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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
ノート
印刷プレビュー

反応式

HRID 858052 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 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

生成物 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}-amide収率 51%

試薬・触媒・溶媒 1

HCID 1049
Pyridine
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-761d43e066c841d3950b8ba61d1480c1
出典データセット
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07148229B2

反応ノート

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