Water → HCID 19974642, 화합물

HRID 1451641노트

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HRID 1451641 반응식
[C:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[NH:10][C:11]1[CH:19]=[CH:18][C:17]([S:20][CH3:21])=[CH:16][C:12]=1[C:13]([OH:15])=[O:14])([OH:3])=O.O>P(Cl)(Cl)(Cl)=O>[CH3:21][S:20][C:17]1[CH:16]=[C:12]([C:13]([OH:15])=[O:14])[C:11]2[NH:10][C:5]3[C:4](=[CH:9][CH:8]=[CH:7][CH:6]=3)[C:1](=[O:3])[C:19]=2[CH:18]=1

참가 물질

4

반응물 2

HCID 962WaterHCID 19974595HCID 19974595, 화합물

생성물 1

HCID 19974642HCID 19974642, 화합물

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

실험 절차

The product of part (i) above (2 g) in phosphorus oxychloride (6 ml) was heated at reflux for 1 h. The solution was then cooled (to 0°), and water (15 ml) was added slowly. The mixture was then heated at 100° for 10 min and then poured onto cracked ice. The resulting precipitate was filtered off, washed with water, and crystallised from methanol to give the title compound (1.6 g). IR includes peaks at 1690 cm-1 (CO2H) and 1620 cm-1 (CO).

후처리

  1. temperatureat reflux for 1 h
  2. additionwas added slowly
  3. temperatureThe mixture was then heated at 100° for 10 min
  4. additionpoured
  5. filtrationThe resulting precipitate was filtered off
  6. washwashed with water
  7. customcrystallised from methanol

출처 및 근거

ORD 기록
ord-76c77db7d62247a1b4d752a6666c52e5
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05604237

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