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Hydrochloric Acid → HCID 58413207, 화합물

HRID 240615
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HRID 240615 반응식
C[O:2][C:3]([C:5]1[S:32][C:8]2[N:9]=[CH:10][N:11]=[C:12]([NH:13][C:14]3[CH:19]=[CH:18][C:17]([F:20])=[CH:16][C:15]=3[O:21][C@H:22]3[CH2:27][CH2:26][CH2:25][N:24]([S:28]([CH3:31])(=[O:30])=[O:29])[CH2:23]3)[C:7]=2[C:6]=1[CH3:33])=[O:4].[OH-].[Li+].Cl>C1COCC1.O>[F:20][C:17]1[CH:18]=[CH:19][C:14]([NH:13][C:12]2[C:7]3[C:6]([CH3:33])=[C:5]([C:3]([OH:4])=[O:2])[S:32][C:8]=3[N:9]=[CH:10][N:11]=2)=[C:15]([O:21][C@H:22]2[CH2:27][CH2:26][CH2:25][N:24]([S:28]([CH3:31])(=[O:30])=[O:29])[CH2:23]2)[CH:16]=1
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참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 584131414-[4-Fluoro-2-((S)-1-methanesulfonyl-piperidin-3-yloxy)-phenylamino]-5-methyl-thieno[2,3-d]pyrimidine-6-carboxylic acid methyl ester

생성물 1

HCID 58413207HCID 58413207, 화합물

시약·촉매·용매 2

HCID 962Water용매2회
HCID 8028
Tetrahydrofuran
용매

실험 절차

4-[4-Fluoro-2-((S)-1-methanesulfonyl-piperidin-3-yloxy)-phenylamino]-5-methyl-thieno[2,3-d]pyrimidine-6-carboxylic acid methyl ester (130 mg) was dissolved in THF (3 ml) and a solution of lithium hydroxide* H2O (60 mg) in water (3 ml) was added. The mixture was stirred for 4 h. HCl (2M) was added to adjusted to pH 5 and the volatile solvent partially removed until crystallization occurred. The solid was collected by filtration. The filter cake was washed with water and was dried to give the desired product.

후처리

  1. customthe volatile solvent partially removed until crystallization
  2. filtrationThe solid was collected by filtration
  3. washThe filter cake was washed with water
  4. customwas dried

출처 및 근거

ORD 기록
ord-8c831527f6824befbea196cd77bd0023
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08648068B2

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