Sodium borohydride → 7-Chloro-2,3-dihydrobenzo[d]isothiazole 1,1-Dioxide

HRID 279761ノート

反応式

HRID 279761 の反応式
[Cl:1][C:2]1[C:10]2[S:9](=[O:12])(=[O:11])[N:8]=[CH:7][C:6]=2[CH:5]=[CH:4][CH:3]=1.[BH4-].[Na+]>C(O)(=O)C>[Cl:1][C:2]1[C:10]2[S:9](=[O:12])(=[O:11])[NH:8][CH2:7][C:6]=2[CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 136863097-Chloro-1,2-benzisothiazole-1,1-dioxide

生成物 1

HCID 136863107-Chloro-2,3-dihydrobenzo[d]isothiazole 1,1-Dioxide収率 97.4%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
0 °C

実験手順

A suspension of 17.9 g of 7-chloro-1,2-benzisothiazole-1,1-dioxide in 180 ml of absolute etnanol was cooled to 0° C. and treated with 3.33 g of sodium borohydride at such a rate that the temperature remained below 5° C. The mixture was warmed to room temperature for 30 minutes, recooled to 0° C. and treated with glacial acetic acid to destroy excess hydride. The mixture was concentrated to dryness, the resulting solid suspended in water, filtered, washed with water and dried in vacuo at 50° C. for 16 hours to give 17.6 g of the title compound as a white powder, m.p. 159°-161° C.

後処理

  1. customremained below 5° C
  2. temperatureThe mixture was warmed to room temperature for 30 minutes
  3. customrecooled to 0° C.
  4. customto destroy excess hydride
  5. concentrationThe mixture was concentrated to dryness
  6. filtrationfiltered
  7. washwashed with water
  8. customdried in vacuo at 50° C. for 16 hours

出典と根拠

ORDレコード
ord-f16e9ff3802142468fbe1ec39030cd25
出典データセット
uspto-grants-1986_05
特許番号
US04586950

反応ノート

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