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

Water → HCID 19008610, 화합물

HRID 1742187
노트
인쇄 미리보기

반응식

HRID 1742187 반응식
[H-].[Na+].[Cl:3][C:4]1[CH:26]=[C:25]([C:27]([F:30])([F:29])[F:28])[CH:24]=[CH:23][C:5]=1[O:6][C:7]1[CH:22]=[CH:21][C:10]2[NH:11][C:12](=[O:20])[CH:13]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[O:14][C:9]=2[CH:8]=1.[CH3:31]I.O>CN(C)C=O>[Cl:3][C:4]1[CH:26]=[C:25]([C:27]([F:28])([F:29])[F:30])[CH:24]=[CH:23][C:5]=1[O:6][C:7]1[CH:22]=[CH:21][C:10]2[N:11]([CH3:31])[C:12](=[O:20])[CH:13]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[O:14][C:9]=2[CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 19008596HCID 19008596, 화합물2회

생성물 1

HCID 19008610HCID 19008610, 화합물수율 48.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매3회

실험 절차

60% Sodium hydride (1.0 g) was suspended in dimethylformamide (hereinafter abbreviated as DMF) (5 ml) and under ice-cooling, a DMF solution (5 ml) of ethyl 7-(2-chloro-4-trifluoromethylphenoxy)-3,4-dihydro-3-oxo-2H-1,4-benzoxazine-2-carboxylate (Compound 1) (0.8 g) was dropwise added thereto, followed by stirring for 10 minutes. Methyl iodide (0.4 g) was then added, the mixture was further stirred for 10 minutes, and to the reaction mixture was added water (20 ml) and the mixture was extracted twice with ethyl acetate (50 ml). The extract was washed with water and then saturated aqueous sodium chloride, and dried over magnesium sulfate. The solvent was then evaporated under a reduced pressure and the residue was purified by silica gel chromatography (eluant: n-hexane/ethyl acetate=3/1) to give 0.4 g of the title compound (colorless oil).

후처리

  1. temperatureunder ice-cooling
  2. stirringthe mixture was further stirred for 10 minutes
  3. extractionthe mixture was extracted twice with ethyl acetate (50 ml)
  4. washThe extract was washed with water
  5. dry with materialsaturated aqueous sodium chloride, and dried over magnesium sulfate
  6. customThe solvent was then evaporated under a reduced pressure
  7. customthe residue was purified by silica gel chromatography (eluant: n-hexane/ethyl acetate=3/1)

출처 및 근거

ORD 기록
ord-24fef3739ba7443ca80f63544d05c527
출처 데이터셋
uspto-grants-1994_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05338719

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트