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Trifluoroacetic acid → 2,2,2-Trifluoro-1-[7-(phenylmethyl)-4,7-diazaspiro[2.5]oct-4-yl]ethanone

HRID 1876609
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HRID 1876609 반응식
[F:1][C:2]([F:7])([F:6])[C:3](O)=[O:4].[CH2:8]([N:15]1[CH2:22][C:19]2([CH2:21][CH2:20]2)[NH:18][CH2:17][CH2:16]1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.C(N(CC)CC)C.C(=O)(O)[O-].[Na+]>C(Cl)(Cl)Cl.C(Cl)Cl>[CH2:8]([N:15]1[CH2:22][C:19]2([CH2:21][CH2:20]2)[N:18]([C:3](=[O:4])[C:2]([F:7])([F:6])[F:1])[CH2:17][CH2:16]1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1
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참가 물질

7

반응물 4

HCID 6422Trifluoroacetic acidHCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 585423257-Benzyl-4,7-diazaspiro[2.5]octane

생성물 1

HCID 585424062,2,2-Trifluoro-1-[7-(phenylmethyl)-4,7-diazaspiro[2.5]oct-4-yl]ethanone수율 102.1%

시약·촉매·용매 2

HCID 6212
Chloroform
용매
HCID 6344Dichloromethane용매

실험 절차

Anhydrous trifluoroacetic acid (8.50 ml, 61.1 mmol) was added dropwise to a methylene chloride (200 ml) solution of the compound (10.3 g, 50.9 mmol) obtained in Step 3 above and triethylamine (17 ml, 122 mmol) with ice cooling and the resulting mixture was stirred at the same temperature for 1 hour. Saturated aqueous sodium bicarbonate solution was added to the reaction mixture, the resulting mixture was diluted with chloroform, washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure to give the title compound (15.5 g, 100%) as a colorless oil.

후처리

  1. washwashed with saturated brine
  2. dry with materialdried over anhydrous sodium sulfate
  3. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-546dd40b1bf6455ba49dfd81afdbaa98
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08309546B2

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