Citric Acid → HCID 59135672, 화합물

HRID 1960317

반응식

HRID 1960317 반응식
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]

참가 물질

8

반응물 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

생성물 1

HCID 59135672HCID 59135672, 화합물수율 76%

시약·촉매·용매 3

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매2회HCID 8857Ethyl Acetate용매

반응 조건

온도
50 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-be3bb0865fd24c32b5488e8599f76ffd
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08410087B2

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