Citric Acid → HCID 59135672、化合物

HRID 1960317

反応式

HRID 1960317 の反応式
C([O:3][C:4](=[O:36])[CH2:5][N:6]1[CH2:11][CH2:10][N:9]([CH2:12][C:13]2[S:17][C:16]([C:18]3[NH:19][C:20]4[C:25]([CH:26]=3)=[CH:24][CH:23]=[CH:22][C:21]=4[NH:27][S:28]([C:31]3[S:32][CH:33]=[CH:34][CH:35]=3)(=[O:30])=[O:29])=[N:15][CH:14]=2)[CH2:8][CH2:7]1)C.[OH-].[Na+].C(O)(=O)CC(CC(O)=O)(C(O)=O)O.[Cl-].[Na+]>O1CCCC1.C(OCC)(=O)C.CO>[S:32]1[CH:33]=[CH:34][CH:35]=[C:31]1[S:28]([NH:27][C:21]1[CH:22]=[CH:23][CH:24]=[C:25]2[C:20]=1[NH:19][C:18]([C:16]1[S:17][C:13]([CH2:12][N:9]3[CH2:10][CH2:11][N:6]([CH2:5][C:4]([OH:36])=[O:3])[CH2:7][CH2:8]3)=[CH:14][N:15]=1)=[CH:26]2)(=[O:29])=[O:30]

参加物

8

反応物 4

HCID 311Citric AcidHCID 5234Sodium ChlorideHCID 14798Sodium HydroxideHCID 59136017ethyl {4-[(2-{7-[(2-thienylsulfonyl)amino]-1H-indol-2-yl}-1,3-thiazol-5-yl)methyl]piperazin-1-yl}acetate

生成物 1

HCID 59135672HCID 59135672、化合物収率 76%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒2 回HCID 8857Ethyl Acetate溶媒

反応条件

温度
50 °C

実験手順

To a solution of ethyl{4-[(2-{7-[(2-thienylsulfonyl)amino]-1H-indol-2-yl}-1,3-thiazol-5-yl)methyl]piperazin-1-yl}acetate (0.500 g) in a mixed solvent of tetrahydrofuran (15 ml) and methanol (5 ml) was added 2N aqueous sodium hydroxide solution (1.5 ml), and the mixture was stirred at 50° C. for 2 hr. 10% Aqueous citric acid solution, ethyl acetate, sodium chloride and tetrahydrofuran were successively added to the reaction solution, and the precipitated crystals were collected by filtration, washed with ethyl acetate, and dried to give the title compound (0.360 g, yield 76%) as colorless crystals.

後処理

  1. filtrationthe precipitated crystals were collected by filtration
  2. washwashed with ethyl acetate
  3. customdried

出典と根拠

ORDレコード
ord-be3bb0865fd24c32b5488e8599f76ffd
出典データセット
uspto-grants-2013_04
特許番号
US08410087B2

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