Chloroform → 4-chloro-N-methylbenzothiazolone

HRID 847802

반응식

HRID 847802 반응식
[Cl:1][C:2]1[C:7]2[N:8]=[C:9](OC)S[C:6]=2[CH:5]=[CH:4][CH:3]=1.[S:13]([O:18]C)(OC)(=O)=O.[CH:20](Cl)(Cl)Cl>>[Cl:1][C:2]1[C:7]2[N:8]([CH3:9])[CH2:20][S:13](=[O:18])[C:6]=2[CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 3

HCID 6212ChloroformHCID 6497Dimethyl SulfateHCID 41419694-Chloro-2-methoxybenzothiazole

생성물 1

HCID 696450104-chloro-N-methylbenzothiazolone수율 99.7%

반응 조건

온도
150 °C

실험 절차

A mixture of 4-chloro-2-methoxybenzothiazole (3.00 g, 0.015 mole) and dimethyl sulfate (95 mg, 7.5×10-4 mole) was heated at 150° C. for 3 hours with stirring. After cooling, the reaction mass was dissolved in chloroform, and the chloroform layer was washed with an aqueous solution saturated with sodium carbonate and then with water. The solvent was removed under reduced pressure to obtain 2.99 g of 4-chloro-N-methylbenzothiazolone as white crystals. Yield 99.7%, purity 99.0%, m.p. 130°-132° C.

후처리

  1. temperatureAfter cooling
  2. washthe chloroform layer was washed with an aqueous solution saturated with sodium carbonate
  3. customThe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-3430b6b0385643a59c87c7ea15694002
출처 데이터셋
uspto-grants-1981_10
특허 번호
US04293702

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