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2-Methyl-2-butene → 5-({2-[4-(2-tert-Butylphenyl)piperazin-1-yl]-2-oxoethyl}sulfanyl)-1,3-dimethyl-1H-pyrazole-4-carboxylic acid

HRID 534877
ノート
印刷プレビュー

反応式

HRID 534877 の反応式
[C:1]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[N:11]1[CH2:16][CH2:15][N:14]([C:17](=[O:29])[CH2:18][S:19][C:20]2[N:24]([CH3:25])[N:23]=[C:22]([CH3:26])[C:21]=2[CH:27]=[O:28])[CH2:13][CH2:12]1)([CH3:4])([CH3:3])[CH3:2].P([O-])(O)(O)=[O:31].[Na+].CC(=CC)C.Cl([O-])=O.[Na+].S([O-])(O)=O.[Na+]>O.C(O)(C)(C)C.O1CCCC1>[C:1]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[N:11]1[CH2:12][CH2:13][N:14]([C:17](=[O:29])[CH2:18][S:19][C:20]2[N:24]([CH3:25])[N:23]=[C:22]([CH3:26])[C:21]=2[C:27]([OH:31])=[O:28])[CH2:15][CH2:16]1)([CH3:4])([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 105532-Methyl-2-buteneHCID 23665763Sodium BisulfiteHCID 23668197Sodium ChloriteHCID 23672064Monosodium phosphateHCID 866633985-({2-[4-(2-tert-butylphenyl)piperazin-1-yl]-2-oxoethyl}sulfanyl)-1,3-dimethyl-1H-pyrazole-4-carbaldehyde

生成物 1

HCID 66792709
5-({2-[4-(2-tert-Butylphenyl)piperazin-1-yl]-2-oxoethyl}sulfanyl)-1,3-dimethyl-1H-pyrazole-4-carboxylic acid
収率 59%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6386tert-Butanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a mixture of 5-({2-[4-(2-tert-butylphenyl)piperazin-1-yl]-2-oxoethyl}sulfanyl)-1,3-dimethyl-1H-pyrazole-4-carbaldehyde (900 mg), sodium dihydrogen phosphate (1.19 g), 2-methyl-2-butene (1.17 mL), tetrahydrofuran (10 mL), tert-butanol (3 mL), and water (1.5 mL) was added sodium chlorite (393 mg) at 0° C. and stirred at room temperature for 1 h. Aqueous sodium hydrogen sulfite was added to the reaction solution, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to provide the title compound (550 mg, 59%) as a colorless solid.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-c4cd66fef43c47e18b2e8f417acef297
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08853215B2

反応ノート

読み込み中…

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