Water → 4-Phenoxy-1,3-benzothiazol-2-amine

HRID 1903731ノート

反応式

HRID 1903731 の反応式
[O:1]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[NH:14][C:15]([NH2:17])=[S:16])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.BrBr.O.[OH-].[Na+]>C(Cl)(Cl)Cl>[NH2:17][C:15]1[S:16][C:10]2[CH:11]=[CH:12][CH:13]=[C:8]([O:1][C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[C:9]=2[N:14]=1

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 24408BromineHCID 1479735(2-Phenoxyphenyl)thiourea

生成物 1

HCID 130970824-Phenoxy-1,3-benzothiazol-2-amine収率 48.7%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

To a mixture of 1-(2-phenoxyphenyl)thiourea (53.4 g) in chloroform (100 ml) was added dropwise a solution of bromine (35.0 g) in chloroform (50 ml) with stirring under ice-cooling during 40 minutes. After refluxing for 1 hour and 40 minutes, the mixture was cooled to ambient temperature. To the resultant mixture was added water and then the mixture was alkalified with 5% sodium hydroxide aqueous solution. The chloroform layer was washed with water, dried over magnesium sulfate, concentrated under reduced pressure to give crystals, which were recrystallized twice from isopropyl alcohol to give 2-amino-4-phenoxybenzothiazole (25.8 g). mp: 135°-137° C.

後処理

  1. temperaturecooling during 40 minutes
  2. temperatureAfter refluxing for 1 hour and 40 minutes
  3. washThe chloroform layer was washed with water
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customto give crystals, which
  7. customwere recrystallized twice from isopropyl alcohol

出典と根拠

ORDレコード
ord-457d68c90d4740bb86216dacccf78077
出典データセット
uspto-grants-1984_03
特許番号
US04438126

反応ノート

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