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Ammonia → HCID 178477851、化合物

HRID 437937
ノート
印刷プレビュー

反応式

HRID 437937 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[CH2:14][CH2:13][C:9]3[S:10][CH:11]=[CH:12][C:8]=3[C:7](=[N:15]O)[C:6]=2[CH:17]=1.[Cl-].[NH4+:19].N>[Zn].C(O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[CH2:14][CH2:13][C:9]3[S:10][CH:11]=[CH:12][C:8]=3[CH:7]([N:15]=[C:5]3[CH2:6][CH2:17][CH2:2][CH2:3][CH2:4][NH:19]3)[C:6]=2[CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 222AmmoniaHCID 25517Ammonium ChlorideHCID 86734897HCID 86734897、化合物

生成物 1

HCID 178477851HCID 178477851、化合物

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 702Ethanol溶媒

実験手順

80.5 g of 6-chloro-9,10-dihydro-4-hydroxyimino-4H-benzo-[4,5]cyclohepta[1,2-b]thiophene, 105 g of zinc dust and 14 g of ammonium chloride are stirred with 1750 ml of 25% ammonia solution and 350 ml of ethanol for 3 hours at the boiling temperature. Upon cooling to room temperature, the undissolved portion is filtered off and is washed with benzene. 200 ml of concentrated caustic soda solution are added to the filtrate which is extracted with a mixture of ether/benzene 1:1. The organic phase is washed with saturated common salt solution, dried over magnesium sulphate and the solvent is removed by evaporation. The remaining 4-amino-6-chloro-9,10-dihydro-4H-benzo[4,5]cyclohepta[1,2-b]thiophene is converted in ethanol into the hydrochloride. M.Pt. decomp. from 234°.

後処理

  1. filtrationthe undissolved portion is filtered off
  2. washis washed with benzene
  3. addition200 ml of concentrated caustic soda solution are added to the filtrate which
  4. extractionis extracted with a mixture of ether/benzene 1:1
  5. washThe organic phase is washed with saturated common salt solution
  6. dry with materialdried over magnesium sulphate
  7. customthe solvent is removed by evaporation
  8. customfrom 234°

出典と根拠

ORDレコード
ord-0b95675c725a458e8768c19f50042fb3
出典データセット
uspto-grants-1977_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04032640

反応ノート

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