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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Ethyl Acetate → 5-chloro-1,3-dimethyl-1H-pyrazole-4-sulfonic acid {4-[1,3-dimethyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-ylmethyl]-phenyl}-amide

HRID 858052
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인쇄 미리보기

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HRID 858052 반응식
[NH2:1][C:2]1[CH:21]=[CH:20][C:5]([CH2:6][C:7]2[NH:15][C:14]3[C:13](=[O:16])[N:12]([CH3:17])[C:11](=[O:18])[N:10]([CH3:19])[C:9]=3[N:8]=2)=[CH:4][CH:3]=1.[Cl:22][C:23]1[N:27]([CH3:28])[N:26]=[C:25]([CH3:29])[C:24]=1[S:30](Cl)(=[O:32])=[O:31].C(OCC)(=O)C>N1C=CC=CC=1>[CH3:17][N:12]1[C:13](=[O:16])[C:14]2[NH:15][C:7]([CH2:6][C:5]3[CH:20]=[CH:21][C:2]([NH:1][S:30]([C:24]4[C:25]([CH3:29])=[N:26][N:27]([CH3:28])[C:23]=4[Cl:22])(=[O:31])=[O:32])=[CH:3][CH:4]=3)=[N:8][C:9]=2[N:10]([CH3:19])[C:11]1=[O:18]
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참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 2252288-(4-Aminobenzyl)-1,3-dimethyl-3,7-dihydro-1h-purine-2,6-dioneHCID 27771265-chloro-1,3-dimethyl-1H-pyrazole-4-sulfonyl chloride

생성물 1

HCID 103449845-chloro-1,3-dimethyl-1H-pyrazole-4-sulfonic acid {4-[1,3-dimethyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-ylmethyl]-phenyl}-amide수율 51%

시약·촉매·용매 1

HCID 1049
Pyridine
용매

실험 절차

To a solution of crude 8-(4-amino-benzyl)-1,3-dimethyl-3,7-dihydro-purine-2,6-dione (0.2 mmol) in pyridine (2 mL) at 0° C. was added 5-chloro-1,3-dimethyl-1H-pyrazole-4-sulfonyl chloride (0.2 mmol) and the mixture left to stir and warm slowly to ambient temperature overnight. The reaction mixture was poured into ethyl acetate, washed with 1M aqueous hydrochloric acid until all pyridine was removed from the organic phase and the combined aqueous washings back extracted with ethyl acetate. The combined organic layers were dried and concentrated in vacuo to give an orange solid. Purified by trituration with warm acetonitrile to give 5-chloro-1,3-dimethyl-1H-pyrazole-4-sulfonic acid {4-[1,3-dimethyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-ylmethyl]-phenyl}-amide as a pale orange solid (51%); EI-HRMS m/e calculated for C19H20ClN7O4S (M+) 477.0986, found 477.0994.

후처리

  1. waitthe mixture left
  2. washwashed with 1M aqueous hydrochloric acid until all pyridine
  3. customwas removed from the organic phase
  4. extractionthe combined aqueous washings back extracted with ethyl acetate
  5. customThe combined organic layers were dried
  6. concentrationconcentrated in vacuo
  7. customto give an orange solid
  8. customPurified by trituration with warm acetonitrile

출처 및 근거

ORD 기록
ord-761d43e066c841d3950b8ba61d1480c1
출처 데이터셋
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07148229B2

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