Chloroform → 4-chloro-N-methylbenzothiazolone

HRID 847802

反応式

HRID 847802 の反応式
[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

参加物

4

反応物 3

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

生成物 1

HCID 696450104-chloro-N-methylbenzothiazolone収率 99.7%

反応条件

温度
150 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3430b6b0385643a59c87c7ea15694002
出典データセット
uspto-grants-1981_10
特許番号
US04293702

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