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

Methyl iodide → HCID 88151531, 화합물

HRID 324501
노트
인쇄 미리보기

반응식

HRID 324501 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[CH:15]([C:16]3[C:17]([S:23]C)=[N:18][C:19](=[O:22])[NH:20][CH:21]=3)[C:10]3[N:11]=[C:12]([CH3:14])[S:13][C:9]=3[CH:8]=[CH:7][C:6]=2[CH:25]=1.CI.[CH3:28]C(C)([O-])C.[K+]>O1CCCC1.CN(C)C=O.C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[CH:15]([C:16]3[C:17](=[S:23])[NH:18][C:19](=[O:22])[N:20]([CH3:28])[CH:21]=3)[C:10]3[N:11]=[C:12]([CH3:14])[S:13][C:9]=3[CH:8]=[CH:7][C:6]=2[CH:25]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 6328Methyl iodideHCID 23665647Potassium tert-butoxideHCID 178503574HCID 178503574, 화합물

생성물 1

HCID 88151531HCID 88151531, 화합물

시약·촉매·용매 3

HCID 6228Dimethylformamide용매HCID 8028Tetrahydrofuran용매
HCID 8857
Ethyl Acetate
용매

실험 절차

A solution of the product of example 39 step (i) (0.1 g) together with methyl iodide (0.040 ml) and a 1M solution of potassium tert-butoxide in tetrahydrofuran (0.52 ml) in N,N-dimethylformamide (10 ml) was heated at 80° C. for 2 h. The reaction mixture was cooled, diluted with ethyl acetate and washed with saturated aqueous ammonium chloride and brine. The organic phase was dried over magnesium sulphate, filtered and evaporated. The crude product was purified by chromatography eluting with 5% ethanol in ethyl acetate to give a yellow oil (86 mg). This material was dissolved in a saturated blue solution of sodium hydrosulphide in N,N-dimethylformamide (3 ml) and heated at 80° C. for 3 h. The reaction mixture was cooled, diluted with dichloromethane and washed with water. The organic phase was dried over magnesium sulphate, filtered and evaporated. The crude product was purified by chromatography eluting with 30% isohexane in ethyl acetate to give the title compound as a yellow solid.

후처리

  1. temperatureThe reaction mixture was cooled
  2. washwashed with saturated aqueous ammonium chloride and brine
  3. dry with materialThe organic phase was dried over magnesium sulphate
  4. filtrationfiltered
  5. customevaporated
  6. customThe crude product was purified by chromatography
  7. washeluting with 5% ethanol in ethyl acetate

출처 및 근거

ORD 기록
ord-efd569c4efad40118f7a331b419c65ac
출처 데이터셋
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06218376B1

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트