HCID 21973112, 화합물 → 4-((3,5-Bis(trifluoromethyl)benzyloxy)methyl)-4-phenylazepane

HRID 11218

반응식

HRID 11218 반응식
[F:1][C:2]([F:31])([F:30])[C:3]1[CH:4]=[C:5]([CH:23]=[C:24]([C:26]([F:29])([F:28])[F:27])[CH:25]=1)[CH2:6][O:7][CH2:8][C:9]1([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:15][CH2:14][CH2:13][NH:12][C:11](=O)[CH2:10]1>C(OCC)C>[F:30][C:2]([F:1])([F:31])[C:3]1[CH:4]=[C:5]([CH:23]=[C:24]([C:26]([F:29])([F:28])[F:27])[CH:25]=1)[CH2:6][O:7][CH2:8][C:9]1([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:15][CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1

참가 물질

3

반응물 1

HCID 21973112HCID 21973112, 화합물

생성물 1

HCID 116261604-((3,5-Bis(trifluoromethyl)benzyloxy)methyl)-4-phenylazepane

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
65 °C

실험 절차

The mixture of Isomer A of 4-((3,5-bis(trifluoromethyl)benzyloxy)methyl)-4-phenylazepan-2-one (90 mg, 0.20 mmol) in borone.THF complex solution (1.5 M in diethyl ether, 1.08 mL) was stirred at room temperature overnight and then at 65° C. for 1 hr. After cooling down, the mixture was concentrated under vacuum and methanol (0.4 mL) and 1N HCl solution (0.4 mL) was added and the mixture was stirred at 65° C. for 2 hr. After cooling down, the mixture was concentrated under vacuum and neutralized with 1N NaOH solution and extracted with dichloromethane 3 times. The combined organic layers were dried over magnesium sulfate, filtered and concentrated under vacuum to give the product as a clear colorless sticky oil (quantitative yield).

후처리

  1. temperatureAfter cooling down
  2. concentrationthe mixture was concentrated under vacuum and methanol (0.4 mL) and 1N HCl solution (0.4 mL)
  3. additionwas added
  4. temperatureAfter cooling down
  5. concentrationthe mixture was concentrated under vacuum
  6. extractionextracted with dichloromethane 3 times
  7. dry with materialThe combined organic layers were dried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-f97e407b89e84fd9945ecbbef00955b6
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07098203B2

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