Hydrochloric Acid → HCID 178505461、化合物

HRID 555814ノート

反応式

HRID 555814 の反応式
[F:1][C:2]1[CH:3]=[C:4](N)[C:5]([NH2:8])=[CH:6][CH:7]=1.[C:10]([S-:15])(=[S:14])OCC.[K+].O.Cl>CN(C=O)C>[F:1][C:2]1[CH:7]=[CH:6][C:5]2[N:8]=[C:10]([SH:15])[S:14][C:4]=2[CH:3]=1

参加物

6

反応条件

温度
95 °C

実験手順

4-Fluorobenzene-1,2-diamine (10.0 g, 0.077 mol) and potassium O-ethyl carbonodithioate (37.1 g, 0.234 mol) were dissolved in dry DMF (150 mL) under nitrogen and heated to 95° C. for 12 h. The reaction was cooled to RT and 200 mL water was added followed by addition of 5N HCl to get precipitates. After stirring for 1 h, the precipitates were collected by filtration, washed with water and dried under vacuum for 2 h. The crude compound was then washed with chloroform and dried to give 6-fluorobenzo[d]thiazole-2-thiol as yellow solid.

後処理

  1. temperatureThe reaction was cooled to RT
  2. customto get
  3. customprecipitates
  4. filtrationthe precipitates were collected by filtration
  5. washwashed with water
  6. customdried under vacuum for 2 h
  7. washThe crude compound was then washed with chloroform
  8. customdried

出典と根拠

ORDレコード
ord-13c7f6e11af743ab90fc114837dfcdf6
出典データセット
uspto-grants-2011_11
特許番号
US08053438B2

反応ノート

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