HCID 21973112、化合物 → 4-((3,5-Bis(trifluoromethyl)benzyloxy)methyl)-4-phenylazepane

HRID 11218

反応式

HRID 11218 の反応式
[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

参加物

3

反応物 1

HCID 21973112HCID 21973112、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
65 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-f97e407b89e84fd9945ecbbef00955b6
出典データセット
uspto-grants-2006_08
特許番号
US07098203B2

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