2-Hydrazinylidene-1,2-diphenylethanone → HCID 12688534、化合物

HRID 1732649ノート

反応式

HRID 1732649 の反応式
[C:1]1([C:7](=[N:16][NH2:17])[C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:18]1([S:24]([CH2:27][C:28](OCC)=[O:29])(=[O:26])=[O:25])[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.[O-]CC.[Na+]>C(O)C>[C:18]1([S:24]([C:27]2[C:28](=[O:29])[NH:17][N:16]=[C:7]([C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)[C:8]=2[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)(=[O:25])=[O:26])[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1

参加物

5

反応物 3

HCID 792892-Hydrazinylidene-1,2-diphenylethanoneHCID 82078Ethyl (phenylsulphonyl)acetateHCID 2723922Sodium ethoxide

生成物 1

HCID 12688534HCID 12688534、化合物収率 34%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Benzilmonohydrazone (20.3 g) and ethyl α-phenylsulfonylacetate (22.8 g) were charged to a dry reaction flask in absolute ethanol (250 ml). With stirring, sodium ethoxide (6.8 g) was added portionwise When addition was complete, the reaction was heated to reflux for 12 hours. During this time, a 10 percent excess (2.3 g) of the ester was added. The cooled solution was quenched in an equal volume of water and concentrated HCl was added to precipitate a solid. The product was filtered from the cold mixture and recrystallized from ethanol to obtain the title compound as a white solid (34 percent yield), m.p. 254°-256° C.

後処理

  1. additionWhen addition
  2. temperaturethe reaction was heated
  3. temperatureto reflux for 12 hours
  4. customThe cooled solution was quenched in an equal volume of water and concentrated HCl
  5. additionwas added
  6. customto precipitate a solid
  7. filtrationThe product was filtered from the cold mixture
  8. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-a19b5ef609e84c208cffcf290743f1b9
出典データセット
uspto-grants-1980_12
特許番号
US04238490

反応ノート

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