Sulfuryl chloride → 2,5-Dichloro-1,3-benzothiazole
反応式
S(Cl)([Cl:4])(=O)=O.[Cl:6][C:7]1[CH:8]=[CH:9][C:10]2[S:14][C:13](S)=[N:12][C:11]=2[CH:16]=1>>[Cl:4][C:13]1[S:14][C:10]2[CH:9]=[CH:8][C:7]([Cl:6])=[CH:16][C:11]=2[N:12]=1参加物
3
実験手順
Sulfuryl chloride (10 mL) was added to 5-chloro-2-mercaptobenzothiazole at 0° C. After complete addition, the reaction mixture was allowed to warm to rt. After 2 h, the reaction mixture was poured into ice water (100 mL). This was allowed to warm to rt and was extracted with EtOAc (3×). The combined organics were dried over Na2SO4, filtered, and concentrated under reduced pressure. The material was used without further purification. LC-MS: RT=10.03 min., compound does not ionize.
後処理
- additionAfter complete addition
- temperatureto warm to rt
- extractionwas extracted with EtOAc (3×)
- dry with materialThe combined organics were dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe material was used without further purification
出典と根拠
- ORDレコード
- ord-00391b8ed3914bf587955f8c08157b7d
- 出典データセット
- uspto-grants-2016_08
- 特許番号
- US09428522B2
反応ノート
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