Triethylamine → 4-[3-[5-[4-[(3-Fluorophenyl)sulfonyl]piperazin-1-yl]pentyl]-2,5-dihydro-4-methyl-2,5-dioxo-1H-pyrrol-1-yl]-2-(trifluoromethyl)benzonitrile

HRID 982669

反応式

HRID 982669 の反応式
C(N(CC)CC)C.[F:8][C:9]1[CH:10]=[C:11]([S:15](Cl)(=[O:17])=[O:16])[CH:12]=[CH:13][CH:14]=1.[CH3:19][C:20]1[C:21](=[O:49])[N:22]([C:37]2[CH:44]=[CH:43][C:40]([C:41]#[N:42])=[C:39]([C:45]([F:48])([F:47])[F:46])[CH:38]=2)[C:23](=[O:36])[C:24]=1[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][N:30]1[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]1>O1CCCC1.C(OCC)(=O)C>[F:8][C:9]1[CH:10]=[C:11]([S:15]([N:33]2[CH2:34][CH2:35][N:30]([CH2:29][CH2:28][CH2:27][CH2:26][CH2:25][C:24]3[C:23](=[O:36])[N:22]([C:37]4[CH:44]=[CH:43][C:40]([C:41]#[N:42])=[C:39]([C:45]([F:46])([F:47])[F:48])[CH:38]=4)[C:21](=[O:49])[C:20]=3[CH3:19])[CH2:31][CH2:32]2)(=[O:17])=[O:16])[CH:12]=[CH:13][CH:14]=1

参加物

6

実験手順

0.2 ml of a solution of triethylamine in tetrahydrofuran (1.5 mol/l) and 8 mg of 3-fluorophenylsulfonyl chloride in 0.4 ml of tetrahydrofuran were added to a solution of 9 mg of 4-[2,5-dihydro-3-methyl-2,5-dioxo-4-[5-(piperazin-1-yl)pentyl]-1H-pyrrol-1-yl]-2-(trifluoromethyl)benzonitrile in 0.4 ml of tetrahydrofuran, and the mixture was stirred for 8 hours at room temperature. For working-up, the reaction mixture was diluted with ethyl acetate and washed with semi-saturated sodium bicarbonate solution. After the organic phase was concentrated by evaporation, it was chromatographed with methanol/dichloromethane on silica gel, and 6 mg of the title compound was thus obtained as a white solid.

後処理

  1. washwashed with semi-saturated sodium bicarbonate solution
  2. concentrationAfter the organic phase was concentrated by evaporation, it
  3. customwas chromatographed with methanol/dichloromethane on silica gel, and 6 mg of the title compound
  4. customwas thus obtained as a white solid

出典と根拠

ORDレコード
ord-c5bb8c68b09d44b2801ece83c4794984
出典データセット
uspto-grants-2005_03
特許番号
US06861432B2

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