Water → 7-Nitro-4-hydroxy-1,2-benzisothiazole

HRID 1449116ノート

反応式

HRID 1449116 の反応式
Cl[C:2]1[C:7]2[CH:8]=[N:9][S:10][C:6]=2[C:5]([N+:11]([O-:13])=[O:12])=[CH:4][CH:3]=1.[OH-].[Na+].O.S(=O)(=O)(O)[OH:18]>C(O)C>[N+:11]([C:5]1[C:6]2[S:10][N:9]=[CH:8][C:7]=2[C:2]([OH:18])=[CH:3][CH:4]=1)([O-:13])=[O:12]

参加物

6

反応物 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 124306574-Chloro-7-nitro-1,2-benzisothiazole

生成物 1

HCID 1357653737-Nitro-4-hydroxy-1,2-benzisothiazole収率 86%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

43 g of 4-chloro-7-nitro-1,2-benzisothiazole and 16 g of sodium hydroxide powder in 400 ml of ethanol are stirred for 1 hour at 70° C. When the mixture has cooled, 500 ml of water are added, the batch is neutralized with dilute sulfuric acid whilst cooling with ice, and the product which has precipitated is filtered off. The filter cake is then washed with a little ice-cold methanol, and dried. 34 g (86% of theory) of 7-nitro-4-hydroxy-1,2-benzisothiazole are obtained, melting at 284° C. (with decomposition) after one recrystallization from n-butanol.

後処理

  1. temperatureWhen the mixture has cooled
  2. temperaturewhilst cooling with ice
  3. customthe product which has precipitated
  4. filtrationis filtered off
  5. washThe filter cake is then washed with a little ice-cold methanol
  6. customdried

出典と根拠

ORDレコード
ord-1450cd4b526b4bcebb170dbd97b1982f
出典データセット
uspto-grants-1980_02
特許番号
US04189433

反応ノート

読み込み中…