2-Hydrazinylidene-1,2-diphenylethanone → HCID 12688534, 화합물

HRID 1732649노트

반응식

HRID 1732649 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 12688534HCID 12688534, 화합물수율 34%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a19b5ef609e84c208cffcf290743f1b9
출처 데이터셋
uspto-grants-1980_12
특허 번호
US04238490

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