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Hydrochloric Acid → (2-Amino-5-chloro-phenyl)-(1-methyl-[1,2,3]triazol-4-yl)methanone

HRID 29513
ノート
印刷プレビュー

反応式

HRID 29513 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N+:16]([O-])=O)=[C:6]([C:8]([C:10]2[N:11]=[N:12][N:13]([CH3:15])[CH:14]=2)=[O:9])[CH:7]=1.Cl>CO>[NH2:16][C:5]1[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][C:6]=1[C:8]([C:10]1[N:11]=[N:12][N:13]([CH3:15])[CH:14]=1)=[O:9]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 59788741(5-Chloro-2-nitro-phenyl)-(1-methyl-[1,2,3]triazol-4-yl)-methanone

生成物 1

HCID 59788730(2-Amino-5-chloro-phenyl)-(1-methyl-[1,2,3]triazol-4-yl)methanone

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
100 °C

実験手順

To 51 mg (0.19 mmol) of (5-Chloro-2-nitro-phenyl)-(1-methyl-[1,2,3]triazol4-yl)-methanone in 2 ml of methanol were added 0.05 ml of 12M HCl and 200 mg (0.89 mmol) of stannous (II) chloride monohydrate, and the mixture was heated at 100° C. for four hours. The mixture was then cooled to ambient temperature, partitioned between 1M NaOH and ethyl acetate, and the phases were separated. The ethyl acetate phase was washed once each with water and brine, dried over Na2SO4, filtered, and concentrated in vacuo to a solid. The solid was chromatographed to give the title product as a yellow solid.

後処理

  1. temperatureThe mixture was then cooled to ambient temperature
  2. custompartitioned between 1M NaOH and ethyl acetate
  3. customthe phases were separated
  4. washThe ethyl acetate phase was washed once each with water and brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo to a solid
  8. customThe solid was chromatographed

出典と根拠

ORDレコード
ord-3b3bc462b8644c06b04f91289c5000c0
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07420055B2

反応ノート

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