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Iodoethane → Rac-n-(1-ethyl-3-phenyl-piperidin-3-yl)-2-methoxy-4,6-bis-trifluoromethyl-benzamide

HRID 2177534
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HRID 2177534 반응식
[CH3:1][O:2][C:3]1[CH:23]=[C:22]([C:24]([F:27])([F:26])[F:25])[CH:21]=[C:20]([C:28]([F:31])([F:30])[F:29])[C:4]=1[C:5]([NH:7][C:8]1([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH2:13][CH2:12][CH2:11][NH:10][CH2:9]1)=[O:6].[CH2:32](N(C(C)C)C(C)C)[CH3:33].ICC>ClCCl>[CH2:32]([N:10]1[CH2:11][CH2:12][CH2:13][C:8]([NH:7][C:5](=[O:6])[C:4]2[C:20]([C:28]([F:31])([F:29])[F:30])=[CH:21][C:22]([C:24]([F:25])([F:26])[F:27])=[CH:23][C:3]=2[O:2][CH3:1])([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH2:9]1)[CH3:33]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6340IodoethaneHCID 81531DiisopropylethylamineHCID 59438392HCID 59438392, 화합물

생성물 1

HCID 59438481Rac-n-(1-ethyl-3-phenyl-piperidin-3-yl)-2-methoxy-4,6-bis-trifluoromethyl-benzamide수율 58%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 25.mg (0.056 mmol) rac-2-methoxy-N-(3-phenyl-piperidin-3-yl)-4,6-bis-trifluoromethyl-benzamide in 0.25 ml dichloromethane were added 19.7 ul (0.112 mmol) N-ethyldiisopropylamine and finally 6.0 ul (0.0728 mmol) iodoethane. The solution was stirred at room temperature for 20 hours. The solvent was removed in vacuo. The crude product was purified on silica gel (Eluent: Heptane/ethyl acetate 0 to 100%) to provide 15 mg (58%) of the title compound as a colorless oil. MS (m/e): 475.2 (M+H).

후처리

  1. customThe solvent was removed in vacuo
  2. customThe crude product was purified on silica gel (Eluent: Heptane/ethyl acetate 0 to 100%)

출처 및 근거

ORD 기록
ord-763d746e564f4387b84ea70cba43d98c
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09067911B2

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