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Benzisothiazole → 1,2-Benzisothiazole, 5-nitro-

HRID 1681269
ノート
印刷プレビュー

反応式

HRID 1681269 の反応式
[N+:1]([C:4]1[CH:5]=[CH:6][C:7]2[S:11][N:10]=[CH:9][C:8]=2[CH:12]=1)([O-:3])=[O:2].[N+:13]([C:16]1[C:24]2[S:23][N:22]=[CH:21][C:20]=2[CH:19]=[CH:18][CH:17]=1)([O-:15])=[O:14].S1C2C=CC=CC=2C=N1.[N+]([O-])([O-])=O.[K+]>S(=O)(=O)(O)O>[N+:13]([C:12]1[C:8]2[CH:9]=[N:10][S:11][C:7]=2[CH:6]=[CH:5][CH:4]=1)([O-:15])=[O:14].[N+:1]([C:4]1[CH:5]=[CH:6][C:7]2[S:11][N:10]=[CH:9][C:8]=2[CH:12]=1)([O-:3])=[O:2].[N+:13]([C:16]1[C:24]2[S:23][N:22]=[CH:21][C:20]=2[CH:19]=[CH:18][CH:17]=1)([O-:15])=[O:14]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 9225BenzisothiazoleHCID 24434Potassium NitrateHCID 1984101,2-Benzisothiazole, 5-nitro-HCID 1986561,2-Benzisothiazole, 7-nitro-

生成物 3

HCID 1984101,2-Benzisothiazole, 5-nitro-HCID 1986561,2-Benzisothiazole, 7-nitro-
HCID 19387300
HCID 19387300、化合物

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

反応条件

温度
-40 °C

実験手順

P.2 4-Nitrobenzisothiazole, 5-nitrobenzisothiazole and 7-nitrobenzisothiazole 300 g of benzisothiazole are added, with cooling, to 750 ml of concentrated sulfuric acid, the solution is cooled to -40° C., and 227.5 g of potassium nitrate are added in portions, in such a manner that the temperature does not rise above room temperature. After standing at room temperature for 15 hours, the reaction mixture is poured onto ice and the solid portion is filtered off and dried. The product is chromatographed on silica gel with tetrahydrofuran:methylene chloride:hexane 5:10:85. After evaporation, there are isolated from the fractions 5.5% of the theorectical yield of 4-nitrobenzisothiazole, 56.5% of the theoretical yield of 5-nitrobenzisothiazole and 36.8% of the theoretical yield of 7-nitrobenzisothiazole (compounds 16, 11 and 1, Table).

後処理

  1. customdoes not rise above room temperature
  2. additionthe reaction mixture is poured onto ice
  3. filtrationthe solid portion is filtered off
  4. customdried
  5. customThe product is chromatographed on silica gel with tetrahydrofuran:methylene chloride:hexane 5:10:85
  6. customAfter evaporation, there

出典と根拠

ORDレコード
ord-1159bcb776a149679a1797dd68b982ab
出典データセット
uspto-grants-1992_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05169951

反応ノート

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