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

Water → Ethyl 7-{[4-(acetyloxy)nonyl](cyano)amino}heptanoate

HRID 1729911
노트
인쇄 미리보기

반응식

HRID 1729911 반응식
[H-].[Na+].[NH:3]([CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:4]#[N:5].Cl[CH2:18][CH2:19][CH2:20][CH:21]([O:27][C:28](=[O:30])[CH3:29])[CH2:22][CH2:23][CH2:24][CH2:25][CH3:26].O>C1C=CC=CC=1.CN(C)C=O>[C:28]([O:27][CH:21]([CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])[CH2:20][CH2:19][CH2:18][N:3]([CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:4]#[N:5])(=[O:30])[CH3:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 131047161-Chloro-4-acetoxynonaneHCID 21501476Ethyl 7-(cyanoamino)heptanoate

생성물 1

HCID 71444712Ethyl 7-{[4-(acetyloxy)nonyl](cyano)amino}heptanoate

시약·촉매·용매 2

HCID 241Benzene용매2회
HCID 6228
Dimethylformamide
용매

실험 절차

Sodium hydride (57%, in mineral oil) (0.48 g., 0.01 mole) is washed twice with benzene then suspended in benzene (50 ml.) and dimethylformamide (50 ml.). Ethyl 7-cyanamidoheptanoate (1.98 g. 0.01 mole) (Example N, Step 2) is added and the suspension heated on the steam bath for 15 minutes. The reaction mixture is cooled to room temperature, 1-chloro-4-acetoxynonane (2.6 g., 0.01 mole) (Example A, Step 3) is added and then the reaction is heated on the steam bath for 2 hours then stirred 18 hours at room temperature. The reaction is poured into water (300 ml.) and extracted with benzene (3 × 100 ml.). The benzene is washed with brine then dried over sodium sulfate. Removal of the solvent yields an oil which is purified by silica gel chromatography, elution solvent 3% methanol in chloroform, evaporation of the appropriate fraction affords ethyl 7-[N-(4-acetoxynonyl) cyanamido]-heptanoate. The yield is 3.2 g. (83 %).

후처리

  1. temperaturethe suspension heated on the steam bath for 15 minutes
  2. temperaturethe reaction is heated on the steam bath for 2 hours
  3. extractionextracted with benzene (3 × 100 ml.)
  4. washThe benzene is washed with brine
  5. dry with materialthen dried over sodium sulfate
  6. customRemoval of the solvent
  7. customyields an oil which
  8. customis purified by silica gel chromatography, elution solvent 3% methanol in chloroform, evaporation of the appropriate fraction

출처 및 근거

ORD 기록
ord-7f39267595ec464295f68f56c928d005
출처 데이터셋
uspto-grants-1976_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03989749

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트