Acetic Acid → {4-[(2,5-Difluorobenzoyl)-hydrazono]-4-phenylbutyl}-carbamic acid tert-butyl ester

HRID 512875ノート

反応式

HRID 512875 の反応式
[C:1]([O:5][C:6](=[O:19])[NH:7][CH2:8][CH2:9][CH2:10][C:11](=O)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)([CH3:4])([CH3:3])[CH3:2].[F:20][C:21]1[CH:30]=[CH:29][C:28]([F:31])=[CH:27][C:22]=1[C:23]([NH:25][NH2:26])=[O:24].CC(O)=O>CCO>[C:1]([O:5][C:6](=[O:19])[NH:7][CH2:8][CH2:9][CH2:10][C:11](=[N:26][NH:25][C:23](=[O:24])[C:22]1[CH:27]=[C:28]([F:31])[CH:29]=[CH:30][C:21]=1[F:20])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)([CH3:4])([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 27740742,5-DifluorobenzohydrazideHCID 14267858tert-Butyl (4-oxo-4-phenylbutyl)carbamate

生成物 1

HCID 86604829{4-[(2,5-Difluorobenzoyl)-hydrazono]-4-phenylbutyl}-carbamic acid tert-butyl ester収率 101.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of (4-oxo-4-phenylbutyl)-carbamic acid tert-butyl ester (3.2 g, 12.2 mmol) and 2,5-difluorobenzoic acid hydrazide (2.1 g, 12 mmol) in EtOH (40 mL) was added HOAc (0.5 mL). The reaction was then heated to reflux and stirred for 3 days. The reaction mixture was then cooled to room temperature and concentrated to give desired product (5.1 g).

後処理

  1. temperatureThe reaction was then heated
  2. temperatureto reflux
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-31066b2db7c7493a8e04d5b4a0916dfb
出典データセット
uspto-grants-2015_08
特許番号
US09102639B2

反応ノート

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