홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Water → ethyl 7-[N-(4-acetoxynonyl)methanesulfonamido]heptanoate

HRID 258600
노트
인쇄 미리보기

반응식

HRID 258600 반응식
[H-].[Na+].[CH3:3][S:4]([NH:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])(=[O:6])=[O:5].Cl[CH2:20][CH2:21][CH2:22][CH:23]([O:29][C:30](=[O:32])[CH3:31])[CH2:24][CH2:25][CH2:26][CH2:27][CH3:28].O>C1C=CC=CC=1.CN(C)C=O>[C:30]([O:29][CH:23]([CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])[CH2:22][CH2:21][CH2:20][N:7]([CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])[S:4]([CH3:3])(=[O:6])=[O:5])(=[O:32])[CH3:31]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 12150839Ethyl 7-(methanesulfonamido)heptanoateHCID 131047161-Chloro-4-acetoxynonane

생성물 1

HCID 20327690ethyl 7-[N-(4-acetoxynonyl)methanesulfonamido]heptanoate

시약·촉매·용매 2

HCID 241Benzene용매
HCID 6228
Dimethylformamide
용매

실험 절차

Sodium hydride (0.715 g., 0.0298 mole) is suspended in benzene (30 ml.) and dimethylformamide (30 ml.). Ethyl 7-(methanesulfonamido)heptanoate (6.8 g., 0.0271 mole) (Example O, Step 1) is added and the suspension heated on the steam bath for 15 minutes. After cooling to room temperature, 1-chloro-4-acetoxynonane (6.55 g., 0.0298 mole) (Example A, Step 3) is added over 15 minutes and the resulting solution heated on the steam bath for 20 hours. Then the reaction is poured into water (300 ml.) and extracted with ethyl acetate (3× 100 ml.). The organic layer is washed with brine (2× 50 ml.), dried over sodium sulfate then concentrated in vacuo to an oil which is purified by chromatography on silica gel. The silica gel is eluted with 3% methanol in chloroform and evaporation of the appropriate fraction affords ethyl 7-[N-(4-acetoxynonyl)methanesulfonamido]heptanoate. The yield is 6.0 g. (51%).

후처리

  1. temperaturethe suspension heated on the steam bath for 15 minutes
  2. temperaturethe resulting solution heated on the steam bath for 20 hours
  3. extractionextracted with ethyl acetate (3× 100 ml.)
  4. washThe organic layer is washed with brine (2× 50 ml.)
  5. dry with materialdried over sodium sulfate
  6. concentrationthen concentrated in vacuo to an oil which
  7. customis purified by chromatography on silica gel
  8. washThe silica gel is eluted with 3% methanol in chloroform and evaporation of the appropriate fraction

출처 및 근거

ORD 기록
ord-c7841865984b4f8d9922f3b38090cba8
출처 데이터셋
uspto-grants-1977_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04033996

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트