Phosphorus oxychloride → N-(3,4-dichlorostyrylsulfonyl)-3,4-dimethoxybenzamide

HRID 66204

反応式

HRID 66204 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:11]=[CH:12][C:13]=1[Cl:14])[CH:5]=[CH:6][S:7]([NH2:10])(=[O:9])=[O:8].[CH3:15][O:16][C:17]1[CH:18]=[C:19]([CH:23]=[CH:24][C:25]=1[O:26][CH3:27])[C:20](Cl)=[O:21].P(Cl)(Cl)(Cl)=O>>[Cl:1][C:2]1[CH:3]=[C:4]([CH:11]=[CH:12][C:13]=1[Cl:14])[CH:5]=[CH:6][S:7]([NH:10][C:20](=[O:21])[C:19]1[CH:23]=[CH:24][C:25]([O:26][CH3:27])=[C:17]([O:16][CH3:15])[CH:18]=1)(=[O:8])=[O:9]

参加物

4

反応物 3

HCID 24813Phosphorus oxychlorideHCID 77070Veratroyl chlorideHCID 537943803,4-Dichlorostyrylsulfonamide

生成物 1

HCID 54226549N-(3,4-dichlorostyrylsulfonyl)-3,4-dimethoxybenzamide収率 70%

実験手順

A mixture of 3,4-dichlorostyrylsulfonamide (12.6 g., 0.05 mole) and 3,4-dimethoxybenzoyl chloride (11.0 g., 0.055 mole) in 15 ml. of phosphorus oxychloride is heated at steam bath temperature for a period of 30 min. Excess phosphorus oxychloride is removed under reduced pressure and dry benzene added. The benzene is evaporated and the treatment repeated two times. Benzene (50 ml.) is added to the residue thus obtained and the insoluble solid collected providing 14.6 g. (70% yield) of N-(3,4-dichlorostyrylsulfonyl)-3,4-dimethoxybenzamide, m.p. 145°-147° C.

後処理

  1. customExcess phosphorus oxychloride is removed under reduced pressure and dry benzene
  2. additionadded
  3. customThe benzene is evaporated
  4. additionBenzene (50 ml.) is added to the residue
  5. customthus obtained
  6. customthe insoluble solid collected
  7. customproviding 14.6 g

出典と根拠

ORDレコード
ord-d3085db84eba49a1aa3fa73c1acc3e62
出典データセット
uspto-grants-1978_12
特許番号
US04130663

関連ノート

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