Water → HCID 53897658、化合物

HRID 1780009ノート

反応式

HRID 1780009 の反応式
[CH3:1][C:2]([NH:8][C:9](=[O:18])[C:10]1[CH:15]=[C:14]([Cl:16])[CH:13]=[C:12]([Cl:17])[CH:11]=1)([CH3:7])[C:3]([CH2:5]Cl)=[O:4].[C:19]([O-:22])(=[O:21])[CH3:20].[Na+].O>CN(C=O)C>[CH3:1][C:2]([NH:8][C:9](=[O:18])[C:10]1[CH:15]=[C:14]([Cl:16])[CH:13]=[C:12]([Cl:17])[CH:11]=1)([CH3:7])[C:3]([CH2:5][O:22][C:19](=[O:21])[CH3:20])=[O:4]

参加物

5

反応物 3

HCID 962WaterHCID 517045Sodium AcetateHCID 54029353HCID 54029353、化合物

生成物 1

HCID 53897658HCID 53897658、化合物収率 47.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

N-(1',1'-dimethyl-3'-chloroacetonyl)-3,5-dichlorobenzamide (20 gm, 0.065 m) was dissolved in 100 ml of dry DMF and 10.6 gm (0.128 m) of sodium acetate was added. The slurry was blanketed under a nitrogen atmosphere and then heated to 80°-90° C. for 4 days. The reaction mixture was cooled by adding 100 ml of water. The aqueous solution was extracted four times with 10 ml aliquots of methylene chloride. The combined organic extracts were washed with water (3×100 ml) and brine. The solvent was removed, the resulting white solid dried and then recrystallized from an acetone and hexane (about 1:4) mixture to yield 10.2 gm of the product.

後処理

  1. temperatureheated to 80°-90° C. for 4 days
  2. temperatureThe reaction mixture was cooled
  3. extractionThe aqueous solution was extracted four times with 10 ml aliquots of methylene chloride
  4. washThe combined organic extracts were washed with water (3×100 ml) and brine
  5. customThe solvent was removed
  6. customthe resulting white solid dried
  7. customrecrystallized from an acetone and hexane (about 1:4) mixture

出典と根拠

ORDレコード
ord-4df937c9283643c487237277c7f7bbe4
出典データセット
uspto-grants-1997_05
特許番号
US05629346

反応ノート

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