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

Potassium Hydroxide → 4-Methyl-10-(methylthio)-4H-thieno[3,4-b] [1,5]benzodiazepine

HRID 1605908
노트
인쇄 미리보기

반응식

HRID 1605908 반응식
[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[NH:6][C:5](=[S:13])[C:4]2=[CH:14][S:15][CH:16]=[C:3]12.O1CCOC[CH2:18]1.[OH-].[K+].S([O-])(OC)(=O)=O>CO>[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[N:6]=[C:5]([S:13][CH3:18])[C:4]2=[CH:14][S:15][CH:16]=[C:3]12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 14797Potassium HydroxideHCID 312751,4-DioxaneHCID 4694097Methyl sulfate(1-)HCID 125216534,9-Dihydro-4-methyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-thione

생성물 1

HCID 125216604-Methyl-10-(methylthio)-4H-thieno[3,4-b] [1,5]benzodiazepine

시약·촉매·용매 1

HCID 887Methanol
용매
2회

실험 절차

To a stirred suspension of 0.7 g. of 4,9-dihydro-4-methyl-10H-thieno[3,4-b] [1,5] benzodiazepin-10-thione in 10 ml. of dioxane is added dropwise and simultaneously at 30°-40°C., a solution of 0.95 g. of potassium hydroxide in 10 ml. of methanol and 0.8 ml. of methyl sulfate. After addition is complete, the mixture is stirred for 3 hours, diluted with methanol and filtered. The filtrate is concentrated to about 20 ml., diluted with water and extracted with chloroform. The chloroform solution is concentrated to give a solid, which is recrystallized from methanol-water to give orgnae crystals, m.p. 113°-115°C.

후처리

  1. additionTo a stirred suspension of 0.7 g
  2. additionAfter addition
  3. filtrationfiltered
  4. concentrationThe filtrate is concentrated to about 20 ml
  5. addition, diluted with water
  6. extractionextracted with chloroform
  7. concentrationThe chloroform solution is concentrated
  8. customto give a solid, which
  9. customis recrystallized from methanol-water
  10. customto give orgnae crystals, m.p. 113°-115°C.

출처 및 근거

ORD 기록
ord-7659c979b1de4cafb4fac39d309ea425
출처 데이터셋
uspto-grants-1976_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03951981

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트