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

Water → (3s)-3-Methyl-2,3,4,5-tetrahydro-1h-1,4-benzodiazepin-9-amine

HRID 1082055
노트
인쇄 미리보기

반응식

HRID 1082055 반응식
[NH2:1][C:2]1[C:12]2[NH:11][C:10](=O)[C@H:9]([CH3:14])[NH:8][C:7](=O)[C:6]=2[CH:5]=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCOCC1>[CH3:14][C@@H:9]1[NH:8][CH2:7][C:6]2[CH:5]=[CH:4][CH:3]=[C:2]([NH2:1])[C:12]=2[NH:11][CH2:10]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 11095747HCID 11095747, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 11829983(3s)-3-Methyl-2,3,4,5-tetrahydro-1h-1,4-benzodiazepin-9-amine수율 99.5%

시약·촉매·용매 1

HCID 31275
1,4-Dioxane
용매

실험 절차

14.8 g (0.072 mol) of (S)-9-amino-3-methyl-3,4-dihydro-1H-1,4-benzodiazepine-2,5-dione in 455 ml of dioxane are heated at the reflux temperature with stirring for 48 hours in the presence of 17 g of lithium aluminium hydride. The reaction mixture is cooled in an ice bath and then, slowly and successively, 17 ml of water, 17 ml of a 5N sodium hydroxide solution and 45 ml of water are added. The mixture is left stirring for 2 hours at room temperature, filtration is carried out and washing is carried out with hot tetrahydrofuran and with dichloromethane. The organic phase is recovered and is concentrated. There are obtained 12.7 g of product which is used as is in the following stage.

후처리

  1. temperatureThe reaction mixture is cooled in an ice bath
  2. waitThe mixture is left
  3. filtrationfiltration
  4. washwashing
  5. customThe organic phase is recovered
  6. concentrationis concentrated

출처 및 근거

ORD 기록
ord-f85504502baf461f9da5886cb89b7173
출처 데이터셋
uspto-grants-1996_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05589476

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트