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Methyl 5-methoxy-3-oxopentanoate → HCID 178494792、化合物

HRID 636431
ノート
印刷プレビュー

反応式

HRID 636431 の反応式
[C:1]1([S:7]([C:10]2[C:14]([S:15][CH3:16])=[N:13][NH:12][C:11]=2[NH2:17])(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C[O:19][CH2:20][CH2:21][C:22](=O)[CH2:23][C:24]([O:26][CH3:27])=O>C(O)(=O)C>[C:1]1([S:7]([C:10]2[C:14]([S:15][CH3:16])=[N:13][N:12]3[C:20]([OH:19])=[CH:21][C:22]([CH2:23][CH2:24][O:26][CH3:27])=[N:17][C:11]=23)(=[O:9])=[O:8])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 542416Methyl 5-methoxy-3-oxopentanoateHCID 110547174-benzenesulphonyl-5-methylsulphanyl-2H-pyrazol-3-ylamine

生成物 1

HCID 178494792HCID 178494792、化合物収率 61%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 2.69 g (10 mmol) of) 4-benzenesulphonyl-5-methylsulphanyl-2H-pyrazol-3-ylamine and 1.6 g (10 mmol) of methyl 5-methoxy-3-oxo-valerate in 10 ml of acetic acid was heated at reflux for 4 hrs. The reaction solution was evaporated and the residue was partitioned between H2O and CH2Cl2. The aqueous phase was extracted three times with 80 ml of CH2Cl2. The combined organic phases were dried (MgSO4), filtered and evaporated. Chromatography (SiO2, CH2Cl2/MeOH 20:1) yielded 2.40 g (61%) of 3-benzenesulphonyl-5-(2-methoxy-ethyl)-2-methylsulphanyl-pyrazolo[1,5-a]pyrimidin-7-ol as a beige powder.

後処理

  1. temperatureat reflux for 4 hrs
  2. customThe reaction solution was evaporated
  3. customthe residue was partitioned between H2O and CH2Cl2
  4. extractionThe aqueous phase was extracted three times with 80 ml of CH2Cl2
  5. dry with materialThe combined organic phases were dried (MgSO4)
  6. filtrationfiltered
  7. customevaporated

出典と根拠

ORDレコード
ord-a7f256e765f74f1fb1433246f2979beb
出典データセット
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06194410B1

反応ノート

読み込み中…

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