Benzaldehyde → HCID 178469930, 화합물

HRID 223417

반응식

HRID 223417 반응식
[CH:1](=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:9][C:10]1[C:14]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:13][NH:12][N:11]=1>C1(C)C=CC=CC=1>[CH2:1]([NH:9][C:10]1[C:14]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:13][NH:12][N:11]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 240BenzaldehydeHCID 178469928HCID 178469928, 화합물

생성물 1

HCID 178469930HCID 178469930, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

21.2 g of benzaldehyde is added to a suspension of 25 g of 3-amino-4-ethoxycarbonylpyrazole in 200 ml of toluene. The whole is boiled while separating water. In 3 hours a total of 5 ml of water collects. After the toluene has been evaporated, 50 ml of methanol and 50 ml of THF are added and, under cooling, 23 g of NaBH4 is added at 0°-5° C. After 4 hours' at room temperature, the solvent mixture is drawn off; then 200 ml of ice water is added the whole is extracted three times with 150 ml of methylene chloride each time and the extract is dried over Na2SO4. After concentration, an oil remains that is recrystallized from ligroin/toluene; m.p. 99°-100° C.

후처리

  1. customwhile separating water
  2. customAfter the toluene has been evaporated
  3. addition50 ml of methanol and 50 ml of THF are added
  4. temperatureunder cooling
  5. addition23 g of NaBH4 is added at 0°-5° C
  6. waitAfter 4 hours' at room temperature
  7. additionthen 200 ml of ice water is added the whole
  8. extractionis extracted three times with 150 ml of methylene chloride each time
  9. dry with materialthe extract is dried over Na2SO4
  10. concentrationAfter concentration
  11. customthat is recrystallized from ligroin/toluene

출처 및 근거

ORD 기록
ord-2ec90a6fb4714466a6ec45db3520de38
출처 데이터셋
uspto-grants-1982_10
특허 번호
US04354031

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