午夜插插,噜噜噜影院,啪啪伊人网,欧美熟夫,景甜吻戏视频,男人强操性感蕾丝美女视频在线网站,日本美女跳舞视频

Welcome to chemicalbook!
Chinese English Japanese Germany Korea
400-158-6606
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

ChemicalBook CAS DataBase List PENT-4-YNAL (IN DCM 30% W/W)
18498-59-4

PENT-4-YNAL (IN DCM 30% W/W) synthesis

13synthesis methods
-

Yield: 7.18 g (92%)

Reaction Conditions:

with triethylamine in dichloromethane;water;dimethyl sulfoxide

Steps:

I Example I
Example I Pent-4-ynal. To a solution of oxalyl chloride (9.12 mL, 104.6 mmol) dissolved in methylene chloride (200 mL) at -78° C. was added dimethylsulfoxide (14.8 mL, 209.2 mmol) dissolved in methylene chloride (40 mL) over 20 minutes. The reaction solution was kept under a positive pressure of argon until workup. The reaction mixture was stirred for an additional 30 minutes when pent-4-yn-1-ol (8.00 g, 95.1 mmol) dissolved in methylene chloride (80 mL) was added over 10 minutes. Stirring was continued for an additional 60 minutes. Triethylamine (66.2 mL, 475.5 mmol) was added at -78° C. and the reaction mixture was stirred for 60 minutes and then allowed to warm to 10° C. over an additional hour. Water (200 mL) was added and the two layers were separated. The aqueous layer was acidified with 1% aqueous hydrochloric acid (saturated with NaCl) and then back-extracted with additional methylene chloride (3*100 mL). The combined organic layers were washed with 1% hydrochloric acid (in saturated brine solution, 6*100 mL) and 5% sodium bicarbonate solution (2*50 mL). The aqueous extracts were back-extracted with methylene chloride (2*100 mL) and the combined organic extracts were washed with brine (2*50 mL) and dried (MgSO4). The solvent was removed by rotary evaporation (30° C. water bath) to give 7.18 g (92%) of pent-4-ynal as a yellow oil. 1 H NMR (CDCl3): δ9.8 (s, 1H), 2.8-2.3 (m, 4H), 2.0-1.9 (t, 1H); 1R (neat): 3296 (s), 2926, 2848, 1725(s) cm-1; TLC (silica gel, 90% hexane: 10% ethyl acetate) Rf=0.43. 2-(But-3-ynyl)-1,3-dithiane.

References:

Marion Laboratories, Inc. US4877779, 1989, A

PENT-4-YNAL (IN DCM 30% W/W) Related Search: