Potassium Carbonate → HCID 23312131、化合物

HRID 745801

反応式

HRID 745801 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([C:11]2[CH:12]=[C:13]([OH:19])[C:14]([OH:18])=[CH:15][C:16]=2[CH3:17])(=[O:10])=[O:9])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH:27](Br)[C:28]([OH:30])=[O:29]>CN(C)C=O>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([C:11]2[C:16]([CH3:17])=[CH:15][C:14]3[O:18][CH:27]([C:28]([OH:30])=[O:29])[O:19][C:13]=3[CH:12]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 12433Dibromoacetic AcidHCID 23312109HCID 23312109、化合物

生成物 1

HCID 23312131HCID 23312131、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

In a manner analogous to that described in Example 15, 60.0 g of 4-(4-bromophenylsulphonyl)-5-methyl-1,2-benzenediol are reacted in the presence of 120 g of potassium carbonate in 300 ml of dimethylformamide with a solution of 76.2 g of dibromoacetic acid in 100 ml of dimethylformamide. After working up and chromatographic purification in a manner analogous to that described in Example 15 and crystallisation from 1,2-dichloroethane, 5-(4-bromophenylsulphonyl)-6-methyl-1,3-benzodioxole-2-carboxylic acid is obtained in the form of sand-coloured crystals having a melting point of 170°-172.5°.

後処理

  1. customchromatographic purification in a manner analogous to
  2. customthat described in Example 15 and crystallisation from 1,2-dichloroethane

出典と根拠

ORDレコード
ord-cbf23a6c952845489fcf099f6f664760
出典データセット
uspto-grants-1986_07
特許番号
US04600709

関連ノート

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