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HCID 58288264、化合物 → HCID 58288367、化合物

HRID 1476120
ノート
印刷プレビュー

反応式

HRID 1476120 の反応式
C([NH:8][C:9]1[CH:10]=[C:11]([CH2:16][C:17]([CH3:26])([CH3:25])[C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH:12]=[CH:13][C:14]=1[Cl:15])C1C=CC=CC=1>C(OCC)(=O)C.[Pd]>[NH2:8][C:9]1[CH:10]=[C:11]([CH2:16][C:17]([CH3:26])([CH3:25])[C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH:12]=[CH:13][C:14]=1[Cl:15]
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 1

HCID 58288264HCID 58288264、化合物

生成物 1

HCID 58288367HCID 58288367、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8857Ethyl Acetate溶媒

実験手順

2.7 g (about 7.22 mmol) of tert-butyl 3-[3-(benzylamino)-4-chlorophenyl]-2,2-dimethylpropanoate were dissolved in 150 ml of ethyl acetate, and 100 ml of palladium on carbon (10%) were added. The reaction mixture was stirred at RT under an atmosphere of hydrogen at atmospheric pressure overnight. The mixture was then filtered off with suction through kieselguhr, the residue was washed thoroughly with ethyl acetate and the combined filtrate was concentrated. The crude product was purified by chromatography on silica gel (mobile phase cyclohexane/ethyl acetate 10:1→7:1). This gave 1.49 g (72.7% of theory) of the target compound.

後処理

  1. filtrationThe mixture was then filtered off with suction through kieselguhr
  2. washthe residue was washed thoroughly with ethyl acetate
  3. concentrationthe combined filtrate was concentrated
  4. customThe crude product was purified by chromatography on silica gel (mobile phase cyclohexane/ethyl acetate 10:1→7:1)

出典と根拠

ORDレコード
ord-8a4f14008d564648a5633d8d0b159cc3
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09018414B2

反応ノート

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