Ammonium Chloride → HCID 59432334, 화합물

HRID 507021노트

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HRID 507021 반응식
[F:1][C:2]([F:36])([F:35])[C:3]1[CH:4]=[C:5]([CH:28]=[C:29]([C:31]([F:34])([F:33])[F:32])[CH:30]=1)[CH2:6][N:7]([C:26]#[N:27])[CH:8]1[CH2:14][CH2:13][CH2:12][N:11]([C:15]([O:17][CH:18]([CH3:20])[CH3:19])=[O:16])[C:10]2[CH:21]=[CH:22][C:23]([Br:25])=[CH:24][C:9]1=2.[N-:37]=[N+:38]=[N-:39].[Na+].[Cl-].[NH4+]>CN(C)C=O.O.[OH-].[Na+]>[F:36][C:2]([F:1])([F:35])[C:3]1[CH:4]=[C:5]([CH:28]=[C:29]([C:31]([F:32])([F:33])[F:34])[CH:30]=1)[CH2:6][N:7]([C:26]1[N:37]=[N:38][NH:39][N:27]=1)[CH:8]1[CH2:14][CH2:13][CH2:12][N:11]([C:15]([O:17][CH:18]([CH3:20])[CH3:19])=[O:16])[C:10]2[CH:21]=[CH:22][C:23]([Br:25])=[CH:24][C:9]1=2

참가 물질

7

반응물 3

HCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 86615652HCID 86615652, 화합물

생성물 1

HCID 59432334HCID 59432334, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매2회HCID 14798Sodium Hydroxide용매

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온도
110 °C

실험 절차

Add a solution of (+/−)-isopropyl 5-[(3,5-bistrifluoromethylbenzyl)-cyanoamino]-7-bromo-2,3,4,5-tetrahydrobenzo[b]azepine-1-carboxylate in anhydrous N,N-dimethylformamide dropwise to a stirred suspension of sodium azide and ammonium chloride in anhydrous N,N-dimethylformamide and heat the resulting yellow mixture at 110° C. under nitrogen. Dilute the cooled mixture with water and 2 N NaOH and wash with diethyl ether. Acidify with 5 N HCl, collect the precipitate and wash with water to provide the title compound.

후처리

  1. washwash with diethyl ether
  2. customcollect the precipitate
  3. washwash with water

출처 및 근거

ORD 기록
ord-1c60f1aea8bc477fa5d83b2427c6c116
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07786108B2

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