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Water → HCID 19992280, 화합물

HRID 345487
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HRID 345487 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:16]2[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=2)([CH:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)[OH:9])=[CH:4][CH:3]=1.Cl[CH2:24][CH2:25][C:26]([N:28]([CH3:30])[CH3:29])=[O:27].C(=O)([O-])[O-].[Na+].[Na+].O>CN(C)C=O.[I-].[K+]>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:16]2[CH:17]=[CH:18][C:19]([F:22])=[CH:20][CH:21]=2)([OH:9])[CH:10]2[CH2:11][CH2:12][N:13]([CH2:24][CH2:25][C:26]([N:28]([CH3:30])[CH3:29])=[O:27])[CH2:14][CH2:15]2)=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 32690663-chloro-N,N-dimethylpropanamideHCID 11208889Bis(4-fluorophenyl)(piperidin-4-yl)methanol

생성물 1

HCID 19992280HCID 19992280, 화합물수율 100%

시약·촉매·용매 2

HCID 4875Potassium Iodide
촉매
HCID 6228Dimethylformamide용매

실험 절차

A mixture of 10.0 g (0.033 mole) of α,α-bis(4-fluorophenyl)-4-piperidinemethanol, 4.5 g (0.033 mole) of 3-chloro-N,N-dimethylpropanamide, 14.0 g (0.132 mole) of anhydrous sodium carbonate and 0.3 g (0.002 mole) of potassium iodide in 100 ml of N,N-dimethylformamide was heated on a steam bath for 16 h. The mixture was poured into 2 L of water and extracted three times with 500 ml portions of ethyl acetate. The ethyl acetate fractions were combined, washed with water and brine, dried (MgSO4) and concentrated under reduced pressure to give a glass. Upon trituration with petroleum ether (30°-60° C.) the glass solidified to yield 13.2 g (100%) of a yellow solid. A portion of this solid was recrystallized from ethyl ether to give the title compound as a white solid, mp 134°-135° C.

후처리

  1. temperaturewas heated on a steam bath for 16 h
  2. extractionextracted three times with 500 ml portions of ethyl acetate
  3. washwashed with water and brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated under reduced pressure
  6. customto give a glass

출처 및 근거

ORD 기록
ord-4c0a2f555d09421e99c9f7174d63de9d
출처 데이터셋
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05057524

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