Fumaric Acid → HCID 178482471、化合物

HRID 1620520ノート

反応式

HRID 1620520 の反応式
[F:1][C:2]([F:30])([F:29])[C:3]1[CH:24]=[C:23]([C:25]([F:28])([F:27])[F:26])[CH:22]=[CH:21][C:4]=1[CH2:5][N:6]1[CH2:11][CH2:10][CH:9](/[CH:12]=[C:13]2/[C:14]([NH:19][CH3:20])=[N:15][C:16](=[O:18])[S:17]/2)[CH2:8][CH2:7]1.[C:31]([OH:38])(=[O:37])/[CH:32]=[CH:33]/[C:34]([OH:36])=[O:35]>C(O)C>[C:31]([OH:38])(=[O:37])/[CH:32]=[CH:33]/[C:34]([OH:36])=[O:35].[F:30][C:2]([F:1])([F:29])[C:3]1[CH:24]=[C:23]([C:25]([F:27])([F:28])[F:26])[CH:22]=[CH:21][C:4]=1[CH2:5][N:6]1[CH2:11][CH2:10][CH:9](/[CH:12]=[C:13]2/[C:14]([NH:19][CH3:20])=[N:15][C:16](=[O:18])[S:17]/2)[CH2:8][CH2:7]1

参加物

4

反応物 2

HCID 444972Fumaric AcidHCID 178482470HCID 178482470、化合物

生成物 1

HCID 178482471HCID 178482471、化合物収率 68.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

To a solution of (5Z)-5-({1-[2,4-bis(trifluoromethyl)benzyl]piperidin-4-yl}methylidene)-4-(methylamino)-1,3-thiazol-2(5H)-one (765 mg) in ethanol (15 mL) was added a solution of fumaric acid (197 mg) in ethanol (45 mL). The reaction mixture was stirred at room temperature for 1 hr, the solvent was evaporated under reduced pressure, and the residue was washed with ethyl acetate. The obtained powder was recrystallized from ethanol/heptane to give the title compound (662 mg).

後処理

  1. customthe solvent was evaporated under reduced pressure
  2. washthe residue was washed with ethyl acetate
  3. customThe obtained powder was recrystallized from ethanol/heptane

出典と根拠

ORDレコード
ord-19bd6cf1c467445dbf92355161e552ef
出典データセット
uspto-grants-2014_07
特許番号
US08772277B2

反応ノート

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