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Water → tert-butyl 4-({[1-methyl-5-(tritylamino)-1H-pyrazol-4-yl]amino)carbonyl)-1-piperazinecarboxylate

HRID 1247848
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HRID 1247848 반응식
[CH3:1][N:2]1[C:6]([NH:7][C:8]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[C:5]([NH:27][C:28](=O)[O:29]C2C=CC=CC=2)[CH:4]=[N:3]1.C(N(CC)CC)C.[N:44]1([C:50]([O:52][C:53]([CH3:56])([CH3:55])[CH3:54])=[O:51])[CH2:49][CH2:48][NH:47][CH2:46][CH2:45]1.O>CN(C)C=O>[CH3:1][N:2]1[C:6]([NH:7][C:8]([C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)=[C:5]([NH:27][C:28]([N:47]2[CH2:48][CH2:49][N:44]([C:50]([O:52][C:53]([CH3:56])([CH3:55])[CH3:54])=[O:51])[CH2:45][CH2:46]2)=[O:29])[CH:4]=[N:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 143452tert-Butyl piperazine-1-carboxylateHCID 21904567Phenyl [1-methyl-5-(tritylamino)pyrazol-4-yl]carbamate

생성물 1

HCID 21904511tert-butyl 4-({[1-methyl-5-(tritylamino)-1H-pyrazol-4-yl]amino)carbonyl)-1-piperazinecarboxylate수율 85.6%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

To a suspension of phenyl [1-methyl-5-(tritylamino)-1H-pyrazol-4-yl]carbamate (4.6 g) in N,N-dimethylformamide (32 ml) were added triethylamine (1.08 g) and tertbutyl 1-piperazinecarboxylate (1.99 g). The reaction mixture was stirred for 3 hours and poured into water. The mixture was extracted with ethyl acetate, and the organic layer was concentrated in vacuo. The residue was purified by column chromatography on silica gel (ethyl acetate→ethyl acetate:ethanol=20:1) to give tert-butyl 4-({[1-methyl-5-(tritylamino)-1H-pyrazol-4-yl]amino}carbonyl)-1-piperazinecarboxylate (4.7 g)

후처리

  1. extractionThe mixture was extracted with ethyl acetate
  2. concentrationthe organic layer was concentrated in vacuo
  3. customThe residue was purified by column chromatography on silica gel (ethyl acetate→ethyl acetate:ethanol=20:1)

출처 및 근거

ORD 기록
ord-47a6894f0d294bd9a3db2ea86671a279
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07129232B2

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