Sodium hydride → 11-Acetoxyundecane malonic acid ethyl ester dimethylamide

HRID 1534316노트

반응식

HRID 1534316 반응식
[H-].[Na+].[CH3:3][N-:4][CH3:5].[CH2:6]([O:8][C:9](=[O:14])[CH2:10][C:11]([OH:13])=[O:12])[CH3:7].[C:15]([O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29]Br)(=[O:17])[CH3:16]>CN(C)C=O>[CH3:3][N-:4][CH3:5].[CH2:6]([O:8][C:9](=[O:14])[CH2:10][C:11]([OH:13])=[O:12])[CH3:7].[C:15]([O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])(=[O:17])[CH3:16]

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 501616211-Bromoundecyl acetateHCID 86745466Malonic acid ethyl ester dimethylamide

생성물 1

HCID 8674546511-Acetoxyundecane malonic acid ethyl ester dimethylamide수율 79.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
22 °C

실험 절차

A suspension of 0.6 g of sodium hydride and 3 g of malonic acid ethyl ester dimethylamide in 30 ml of dimethylformamide is stirred for an hour at 22° C., mixed with 6.9 g of 1-acetoxy-11-bromoundecane and stirred for 16 hours at 50° C. Then the reaction mixture is stirred in 200 ml of ice water, extracted with ethyl acetate, the organic phase is dried on sodium sulfate and concentrated by evaporation in vacuum. Thus, 5.3 g of 11-acetoxyundecane malonic acid ethyl ester dimethylamide is obtained as light-yellow oil.

후처리

  1. stirringstirred for 16 hours at 50° C
  2. extractionextracted with ethyl acetate
  3. customthe organic phase is dried on sodium sulfate
  4. concentrationconcentrated by evaporation in vacuum

출처 및 근거

ORD 기록
ord-ad44622a941143c684f47fc172f6d028
출처 데이터셋
uspto-grants-1992_02
특허 번호
US05089175

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