Water → 2-({(2-(4-Chlorophenyl)-1,3-thiazol-4-yl)methyl}sulfanyl)-6-(ethyl(methyl)amino)-4-(4-(2-hydroxyethoxy)phenyl)pyridine-3,5-dicarbonitrile

HRID 1621324노트

반응식

HRID 1621324 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[S:9][CH:10]=[C:11]([CH2:13][S:14][C:15]3[C:20]([C:21]#[N:22])=[C:19]([C:23]4[CH:28]=[CH:27][C:26]([O:29][CH2:30][CH2:31][OH:32])=[CH:25][CH:24]=4)[C:18]([C:33]#[N:34])=[CH:17][N:16]=3)[N:12]=2)=[CH:4][CH:3]=1.[CH2:35]([NH:37][CH3:38])[CH3:36].O>C1COCC1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[S:9][CH:10]=[C:11]([CH2:13][S:14][C:15]3[C:20]([C:21]#[N:22])=[C:19]([C:23]4[CH:28]=[CH:27][C:26]([O:29][CH2:30][CH2:31][OH:32])=[CH:25][CH:24]=4)[C:18]([C:33]#[N:34])=[C:17]([N:37]([CH2:35][CH3:36])[CH3:38])[N:16]=3)[N:12]=2)=[CH:6][CH:7]=1

참가 물질

5

실험 절차

At RT, 60 mg (0.11 mmol) of 2-chloro-6-({(2-(4-chlorophenyl)-1,3-thiazol-4-ylmethyl}sulfanyl)-4-(4-(2-hydroxyethoxy)phenyl)pyridine-3,5-dicarbonitrile (Example 2A) and 0.019 ml (0.22 mmol) of N-ethylmethylamine were stirred in 1.5 ml of THF for 30 min. About 15 ml of water were added to the reaction mixture, and the aqueous phase was extracted 3× with ethyl acetate. The combined organic phases were washed once with sodium chloride solution, dried over sodium sulfate, concentrated by evaporation and dried under high vacuum. This gave 63 mg (99% of theory) of the desired target compound.

후처리

  1. extractionthe aqueous phase was extracted 3× with ethyl acetate
  2. washThe combined organic phases were washed once with sodium chloride solution
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated by evaporation
  5. customdried under high vacuum

출처 및 근거

ORD 기록
ord-3e8afb319f8a4d469b0a2065ab2f08da
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772498B2

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