Hydrochloric Acid → 2(3H)-Benzothiazolethione, 6,7-dichloro-

HRID 598514ノート

反応式

HRID 598514 の反応式
[Cl:1][C:2]1[C:3](F)=[C:4]([CH:6]=[CH:7][C:8]=1[Cl:9])[NH2:5].CCO[C:14]([S-:16])=[S:15].[K+].Cl>CN(C)C=O.O>[Cl:9][C:8]1[CH:7]=[CH:6][C:4]2[N:5]=[C:14]([SH:16])[S:15][C:3]=2[C:2]=1[Cl:1]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 2735045Potassium ethylxanthateHCID 27827033,4-Dichloro-2-fluoroaniline

生成物 1

HCID 1785277912(3H)-Benzothiazolethione, 6,7-dichloro-収率 92%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
95 °C

実験手順

A mixture of 1.5 g (8.33 mmol) 3.4-dichloro-2-fluoroaniline and 1.64 g (10.00 mmol) potassium ethylxanthogenate in 8 mL dry N,N-dimethylformamide was heated in a 95° C. oil bath for 5 h. The reaction mixture was cooled to room temperature and diluted with water (25 mL). The mixture was acidified with aqueous HCl 2N. The precipitate was collected by filtration, washed with water and dried to provide 1.8 g (92%) of the title compound as a white solid. MS(m/e): 233.8 (M−H+).

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. filtrationThe precipitate was collected by filtration
  3. washwashed with water
  4. customdried

出典と根拠

ORDレコード
ord-88f96fc5bfa742dfbcd4c125c62a6cc8
出典データセット
uspto-grants-2011_03
特許番号
US07897627B2

反応ノート

読み込み中…