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Ammonium Hydroxide → HCID 23316356, 화합물

HRID 1982393
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HRID 1982393 반응식
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]2[CH2:6][N:7]3[CH:14]=[CH:13][CH:12]=[C:8]3[C:9](=[O:11])[NH:10][C:4]=2[CH:3]=1.[Cl-:17].[Cl-].[Cl-].[Al+3].[OH-].[NH4+]>C(Cl)Cl>[Cl:17][C:13]1[CH:12]=[C:8]2[N:7]([CH:14]=1)[CH2:6][C:5]1[CH:15]=[CH:16][C:2]([Cl:1])=[CH:3][C:4]=1[NH:10][C:9]2=[O:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14923Ammonium HydroxideHCID 6451240Aluminum(III) ChlorideHCID 12595984HCID 12595984, 화합물

생성물 1

HCID 23316356HCID 23316356, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 2.33 g of 8-chloro-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-11-one in 50 mL of methylene chloride is added 5.33 g of aluminum trichloride. The reaction is stirred for 1 hour at room temperature and 0.77 mL (1.2 g) of methanesulfonyl chgloride is added. Stirring is then continued at room temperature overnight. The reaction mixture is basified with 10% ammonium hydroxide and the resulting solid collected by filtration. The solid is dissolved in methylene chloride, the solution is washed with water, dried over magnesium sulfate and evaporated to dryness to yield 2,8-dichloro-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]-benzodiazepin-11-one, which is used without further purification.

후처리

  1. addition0.77 mL (1.2 g) of methanesulfonyl chgloride is added
  2. stirringStirring
  3. waitis then continued at room temperature overnight
  4. filtrationthe resulting solid collected by filtration
  5. dissolutionThe solid is dissolved in methylene chloride
  6. washthe solution is washed with water
  7. dry with materialdried over magnesium sulfate
  8. customevaporated to dryness

출처 및 근거

ORD 기록
ord-e34ed9aff70c4c539bc45a21da9d4fbb
출처 데이터셋
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04596799

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