Bromine → 7-Chloro-4-methoxy-1,3-benzothiazol-2-amine

HRID 2297028노트

반응식

HRID 2297028 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([Cl:9])=[CH:5][C:4]=1[NH:10][C:11]([NH2:13])=[S:12].BrBr>C(Cl)(Cl)Cl>[NH2:13][C:11]1[S:12][C:5]2[C:6]([Cl:9])=[CH:7][CH:8]=[C:3]([O:2][CH3:1])[C:4]=2[N:10]=1

참가 물질

4

반응물 2

HCID 24408BromineHCID 2732660N-(5-Chloro-2-methoxyphenyl)thiourea

생성물 1

HCID 136667137-Chloro-4-methoxy-1,3-benzothiazol-2-amine

시약·촉매·용매 1

HCID 6212Chloroform용매2회

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온도
10 °C

실험 절차

A solution of 1-(2-methoxy-5-chlorophenyl)-2-thiourea (1 mmole) in chloroform (10 mL) was cooled to 10° C. and treated with bromine (2.2 mmole) in chloroform (10 mL). The reaction was stirred at 10° C. for 20 min and at room temperature for 0.5 h. The resulting suspension was heated at reflux for 0.5 h. The precipitate was collected via filtration (washed with CH2Cl2) to give 2-amino-4-methoxy-7-chlorobenzothiazole which was subjected to Steps A, B, C and D of Example 34 to give 2-amino-4-phosphonomethoxy-6-bromo-7-chloro benzothiazole (35.1). mp>220° C.(dec.). Anal. Calcd. for C8H7N2O4PSClBr: C:25.72; H:1.89; N:7.50. Found: C:25.66; H:1.67; N:7.23.

후처리

  1. temperatureThe resulting suspension was heated
  2. temperatureat reflux for 0.5 h
  3. filtrationThe precipitate was collected via filtration (washed with CH2Cl2)

출처 및 근거

ORD 기록
ord-ec44c92bd8164fd0b1bbf2cb0a232271
출처 데이터셋
uspto-grants-2002_12
특허 번호
US06489476B1

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