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Stannous Chloride → 8-Chloro-2-isopropyl-5H-dibenzo[b,e][1,4]diazepin-11-ylamine hydrochloride

HRID 131340
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HRID 131340 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[CH:16]=[CH:15][C:14]([CH:17]([CH3:19])[CH3:18])=[CH:13][C:10]=2[C:11]#[N:12])=[C:4]([N+:20]([O-])=O)[CH:3]=1.[Sn](Cl)Cl>C(O)C.Cl>[ClH:1].[Cl:1][C:2]1[CH:7]=[CH:6][C:5]2[NH:8][C:9]3[CH:16]=[CH:15][C:14]([CH:17]([CH3:19])[CH3:18])=[CH:13][C:10]=3[C:11]([NH2:12])=[N:20][C:4]=2[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 24479Stannous ChlorideHCID 586259132-(4-Chloro-2-nitro-phenylamino)-5-isopropyl-benzonitrile

생성물 1

HCID 1363841438-Chloro-2-isopropyl-5H-dibenzo[b,e][1,4]diazepin-11-ylamine hydrochloride수율 198%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 702Ethanol용매

실험 절차

Heat a solution of 2-(4-chloro-2-nitro-phenylamino)-5-isopropyl-benzonitrile (0.313 g, 0.99 mmol) in ethanol (6 ml) to 60° C. To this is add a solution of tin (II) chloride (0.752 g, 3.96 mmol) in 5.0 N hydrochloric acid (6 ml) and heat the resulting mixture to reflux for 16 hours. Cool the reaction to room temperature and place in a freezer for 16 hours. Collect by filtration the precipitated product s from the solution and to obtain 0.316 g of the title compound (0.98 mmol, 99% yield) as a yellow amorphous solid: Mass Spectrum (m/e): 286(M+1).

후처리

  1. temperatureheat the resulting mixture
  2. temperatureto reflux for 16 hours
  3. temperatureCool
  4. customthe reaction to room temperature
  5. filtrationCollect by filtration the precipitated product s from the solution

출처 및 근거

ORD 기록
ord-982a38d5da114502a2f62dbcc1689042
출처 데이터셋
uspto-grants-2008_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07384934B2

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