Potassium Carbonate → HCID 21453224, 화합물

HRID 436601노트

반응식

HRID 436601 반응식
[CH2:1]([C:4]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:5]=1[OH:11])[CH:2]=[CH2:3].Cl[CH2:13][CH2:14][CH2:15][N:16]1[CH2:32][CH2:31][C:19]2([N:23]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[CH2:22][NH:21][C:20]2=[O:30])[CH2:18][CH2:17]1.C(=O)([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1>[CH2:1]([C:4]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:5]=1[O:11][CH2:13][CH2:14][CH2:15][N:16]1[CH2:17][CH2:18][C:19]2([N:23]([C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=3)[CH2:22][NH:21][C:20]2=[O:30])[CH2:31][CH2:32]1)[CH:2]=[CH2:3]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 113441122-Allyl-4-fluorophenolHCID 21453222HCID 21453222, 화합물

생성물 1

HCID 21453224HCID 21453224, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of 1.5 g of 2-allyl-4-fluorophenol, 3.1 g of 8-(3-chloropropyl)-1-phenyl-4-oxo-1,3,8-triazaspiro[4,5]decane, 0.7 g of potassium carbonate and 40 ml of toluene was heated under reflux for 10 hours. After cooling, the reaction mixture was washed with water, dried over sodium sulfate and evaporated under reduced pressure. The residue was triturated with ether, cooled and filtered to give 8-{3-(2-allyl-4-fluorophenoxy)propyl}-1-phenyl-4-oxo-1,3,8-triazaspiro[4,5]decane, m.p. 110° - 113° C; recrystallized from cyclohexane, m.p. 117° - 117.5° C.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 10 hours
  3. temperatureAfter cooling
  4. washthe reaction mixture was washed with water
  5. dry with materialdried over sodium sulfate
  6. customevaporated under reduced pressure
  7. customThe residue was triturated with ether
  8. temperaturecooled
  9. filtrationfiltered

출처 및 근거

ORD 기록
ord-890635a35dfe40ce913a0d17b80ad267
출처 데이터셋
uspto-grants-1977_02
특허 번호
US04009275

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