Water → HCID 69289967, 화합물

HRID 2415462노트

반응식

HRID 2415462 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 69289967HCID 69289967, 화합물수율 9,987.2%

시약·촉매·용매 1

HCID 8078Cyclohexane용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-42968eb1c465498a9393959c562404a7
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06818767B2

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