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HCID 15547425, 화합물 → HCID 15547426, 화합물

HRID 1385105
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HRID 1385105 반응식
C([O:8][NH:9][C:10]([C:12]1[CH:17]=[CH:16][C:15]([NH:18][C:19]([C:21]2[CH:29]=[C:28]3[C:24]([C:25]([CH2:35][CH3:36])=[N:26][N:27]3[CH:30]3[CH2:34][CH2:33][CH2:32][CH2:31]3)=[CH:23][CH:22]=2)=[O:20])=[CH:14][CH:13]=1)=[O:11])C1C=CC=CC=1>C(OCC)(=O)C.CO.[Pd]>[OH:8][NH:9][C:10]([C:12]1[CH:17]=[CH:16][C:15]([NH:18][C:19]([C:21]2[CH:29]=[C:28]3[C:24]([C:25]([CH2:35][CH3:36])=[N:26][N:27]3[CH:30]3[CH2:34][CH2:33][CH2:32][CH2:31]3)=[CH:23][CH:22]=2)=[O:20])=[CH:14][CH:13]=1)=[O:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 1

HCID 15547425HCID 15547425, 화합물

생성물 1

HCID 15547426HCID 15547426, 화합물수율 49%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 187 mg (0.387 mmol, 1.0 equiv) 1-cyclopentyl-3-ethyl-1H-indazole-6-carboxylic acid (4-benzyloxycarbamoyl-phenyl)-amide and 200 mg 10% Pd/C in 10 mL ethyl acetate and 10 mL methanol was placed on a Parr® hydrogenation appartus and shaken under 30 psi H2 at room temperature for 1 hour. The reaction mixture was filtered through Celite®, and the filtrate concentrated and dried to give a tan solid. Purification on a silica gel column (CH3OH/CH2Cl2 gradient 4%, 10%, 20%, flash) gave 74 mg (49%) of a tan solid: mp 175° C. (dec); HRMS calcd for C22H24N4O3+H: 393.1928. Found: 393.1949.

후처리

  1. filtrationThe reaction mixture was filtered through Celite®
  2. concentrationthe filtrate concentrated
  3. customdried
  4. customto give a tan solid
  5. customPurification on a silica gel column (CH3OH/CH2Cl2 gradient 4%, 10%, 20%, flash)

출처 및 근거

ORD 기록
ord-12812241efe84a71af79837b70e06d0c
출처 데이터셋
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06262040B1

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