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HCID 414534, 화합물 → HCID 178450192, 화합물

HRID 268269
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HRID 268269 반응식
N[CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)=[O:6].[ClH:13].[NH:14]([C:21]1[C:30]2[C:25](=[CH:26][CH:27]=[C:28]3[N:33]=[CH:32][NH:31][C:29]3=2)[N:24]=[C:23]([CH3:34])[CH:22]=1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>C(O)C>[OH2:6].[ClH:13].[C:5]([C:7]1[CH:12]=[CH:11][C:10]([NH:14][C:21]2[C:30]3[C:25](=[CH:26][CH:27]=[C:28]4[N:33]=[CH:32][NH:31][C:29]4=3)[N:24]=[C:23]([CH3:34])[CH:22]=2)=[CH:9][CH:8]=1)(=[O:6])[CH2:4][CH2:3][CH3:2].[C:5]([C:18]1[CH:19]=[CH:20][C:15]([NH:14][C:21]2[C:30]3[C:25](=[CH:26][CH:27]=[C:28]4[N:33]=[CH:32][NH:31][C:29]4=3)[N:24]=[C:23]([CH3:34])[CH:22]=2)=[CH:16][CH:17]=1)(=[O:6])[CH2:4][CH2:3][CH3:2].[ClH:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 414534HCID 414534, 화합물HCID 178428198HCID 178428198, 화합물

생성물 1

HCID 178450192HCID 178450192, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 16.3 g. (0.1 m) of 4-aminobutyrophenone, 21.7 g. (0.1 m) of the compound of Example I, C. and 500 ml. of ethanol was refluxed overnight. The solution was concentrated in vacuo to dryness. The soft, yellow solid was dissolved in 300 ml. of MeOH and filtered. The MeOH filtrate was evaporated to a volume of 50 ml. then chilled. The product was filtered, washed with ether and oven-dried (110°C) to give 24 g. m.p. 209°-230°C. A second recrystallization from MeOH yielded 22 g., m.p. 205°-235°C.

후처리

  1. additionA mixture of 16.3 g
  2. concentrationThe solution was concentrated in vacuo to dryness
  3. dissolutionThe soft, yellow solid was dissolved in 300 ml
  4. filtrationof MeOH and filtered
  5. customThe MeOH filtrate was evaporated to a volume of 50 ml
  6. temperaturethen chilled
  7. filtrationThe product was filtered
  8. washwashed with ether
  9. customoven-dried (110°C)
  10. customto give 24 g
  11. customA second recrystallization from MeOH
  12. customyielded 22 g

출처 및 근거

ORD 기록
ord-df91841f024e439fba321f4dc825b2aa
출처 데이터셋
uspto-grants-1976_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03947434

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