3-(2-Nitro-benzoylamino)-thieno[2,3-c]pyrazole-1,5-dicarboxylic Acid 5-tert-butyl Ester 1-ethyl Ester → 3-(2-Amino-benzoylamino)-thieno[2,3-c]pyrazole-1,5-dicarboxylic Acid 5-tert-butyl Ester 1-ethyl Ester

HRID 549430노트

반응식

HRID 549430 반응식
[CH2:1]([O:3][C:4]([N:6]1[C:10]2[S:11][C:12]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])=[CH:13][C:9]=2[C:8]([NH:21][C:22](=[O:32])[C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=2[N+:29]([O-])=O)=[N:7]1)=[O:5])[CH3:2]>C(OCC)(=O)C.[Pd]>[CH2:1]([O:3][C:4]([N:6]1[C:10]2[S:11][C:12]([C:14]([O:16][C:17]([CH3:20])([CH3:18])[CH3:19])=[O:15])=[CH:13][C:9]=2[C:8]([NH:21][C:22](=[O:32])[C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=2[NH2:29])=[N:7]1)=[O:5])[CH3:2]

참가 물질

4

반응물 1

HCID 577372653-(2-Nitro-benzoylamino)-thieno[2,3-c]pyrazole-1,5-dicarboxylic Acid 5-tert-butyl Ester 1-ethyl Ester

생성물 1

HCID 577372683-(2-Amino-benzoylamino)-thieno[2,3-c]pyrazole-1,5-dicarboxylic Acid 5-tert-butyl Ester 1-ethyl Ester수율 97.2%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8857Ethyl Acetate용매

실험 절차

The suspension of 3-(2-Nitro-benzoylamino)-thieno[2,3-c]pyrazole-1,5-dicarboxylic acid 5-tert-butyl ester 1-ethyl ester (984 mg, 2.136 mmol) and Pd/C 10% (200 mg) in ethyl acetate (AcOEt, 35 mL) was shaken under hydrogen pressure (40 psi) for 10 hours. The solid was filtered on celite, washed with AcOEt and the filtrate was evaporated under vacuum to yield 894 mg (97%) of title compound.

후처리

  1. filtrationThe solid was filtered on celite
  2. washwashed with AcOEt
  3. customthe filtrate was evaporated under vacuum

출처 및 근거

ORD 기록
ord-6b5ccae04b70410aba0c6966315f9acd
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07943654B2

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