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

HRID 598514노트

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HRID 598514 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

반응 조건

온도
95 °C

실험 절차

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+).

후처리

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

출처 및 근거

ORD 기록
ord-88f96fc5bfa742dfbcd4c125c62a6cc8
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07897627B2

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