Water → HCID 69289967、化合物

HRID 2415462ノート

反応式

HRID 2415462 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([CH:13]=[CH:14][CH:15]=1)[NH2:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:16]([O:22][CH2:23][CH3:24])(=[O:21])[CH2:17][C:18]([CH3:20])=O.O.C1(C)C=CC(S(O)(=O)=O)=CC=1.O>C1CCCCC1>[CH2:23]([O:22][C:16](=[O:21])[CH:17]=[C:18]([NH:12][C:11]1[CH:13]=[CH:14][CH:15]=[C:9]([O:8][CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[CH:10]=1)[CH3:20])[CH3:24]

参加物

6

反応物 4

HCID 962WaterHCID 8868Ethyl AcetoacetateHCID 928923-BenzyloxyanilineHCID 521998p-Toluenesulfonic acid monohydrate

生成物 1

HCID 69289967HCID 69289967、化合物収率 9,987.2%

試薬・触媒・溶媒 1

HCID 8078Cyclohexane溶媒

実験手順

20 g (98.4 mmol)of 3-benyloxyaniline, 12.6 ml (0.984 mmol) of ethyl acetoacetate and 0.189 g (1 mmol) of p-toluenesulfonic acid monohydrate in 32 ml of cyclohexane were heated at reflux for 5.5 h in the presence of a water separator funnel. The reaction mixture was cooled to RT, some solid material was filtered off by suction and the filtrate was concentrated in vacuo to give 30.6 g (99%) of the desired 3-(3-benzyloxy-phenylamino)-but-2-enoic acid ethyl ester as a yellow oil. This was used without further purification in the next reaction step.

後処理

  1. filtrationsome solid material was filtered off by suction
  2. concentrationthe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-42968eb1c465498a9393959c562404a7
出典データセット
uspto-grants-2004_11
特許番号
US06818767B2

反応ノート

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