Bentazon → Bentazone ammonium

HRID 482303

反応式

HRID 482303 の反応式
[CH3:1][CH:2]([N:4]1[S:14](=[O:16])(=[O:15])[NH:13][C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:5]1=[O:6])[CH3:3].O.[NH3:18]>ClCCCl>[CH3:3][CH:2]([N:4]1[S:14](=[O:16])(=[O:15])[NH:13][C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:5]1=[O:6])[CH3:1].[NH4+:18]

参加物

4

反応物 2

HCID 2328BentazonHCID 12896473Azane;hydrate

生成物 1

HCID 131720800Bentazone ammonium収率 45.7%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

A solution of 24 g of bentazone (IIa) in 216 g of 1,2-dichloroethane was treated with stirring at 50°-60° C. with 34 g of ammonia water (5% strength solution of ammonia in water). After addition was complete, the aqueous phase was separated off at 50°-60° C. On cooling the aqueous phase, the bentazone-ammonium was deposited in crystalline form. The solid was separated off at 20° C. by filtration and freed from solvent residues under reduced pressure and at 50° C. 11.8 g of bentazone-ammonium (m.p. 180° C.) were obtained. By evaporating the water from the mother liquor under reduced pressure and at 50°-60° C., a further 13.7 g of bentazone-ammonium were obtained.

後処理

  1. additionAfter addition
  2. customthe aqueous phase was separated off at 50°-60° C
  3. temperatureOn cooling the aqueous phase
  4. customThe solid was separated off at 20° C. by filtration
  5. customfreed from solvent residues under reduced pressure and at 50° C

出典と根拠

ORDレコード
ord-46d50470d3c3400fa5fbd4aa28670455
出典データセット
uspto-grants-1998_08
特許番号
US05795983

関連ノート

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