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Acetic Anhydride → N-[3-(4-Hydroxyphenyl)-1-methylpropyl]acetamide

HRID 1260500
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HRID 1260500 반응식
[NH2:1][CH:2]([CH3:12])[CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[CH:7][CH:6]=1.C(N(CC)CC)C.[C:20](OC(=O)C)(=[O:22])[CH3:21]>C(OCC)(=O)C>[OH:11][C:8]1[CH:7]=[CH:6][C:5]([CH2:4][CH2:3][CH:2]([NH:1][C:20](=[O:22])[CH3:21])[CH3:12])=[CH:10][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 97939244-(3-Aminobutyl)phenol

생성물 1

HCID 59956161N-[3-(4-Hydroxyphenyl)-1-methylpropyl]acetamide

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

4-(3-Aminobutyl)phenol (510 mg, 3.087 mmol) and triethylamine (1.3 ml, 9.26 mmol) were dissolved in 30 ml of ethyl acetate. At 0° C., acetic anhydride (029 ml, 3.087 mmol) was added. The cooling bath was removed after 1 h. The reaction mixture was concentrated, and the residue was purified by preparative HPLC (PR18, acetonitrile/water 0.1% TFA). Yield: 472 mg (74%) of N-[3-(4-hydroxyphenyl)-1-methylpropyl]acetamide, M+H+: 208.14 and 54 mg (7%) of 4-(3-acetylaminobutyl)phenyl acetate, M+H+: 250.13.

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후처리

  1. customThe cooling bath was removed after 1 h
  2. concentrationThe reaction mixture was concentrated
  3. customthe residue was purified by preparative HPLC (PR18, acetonitrile/water 0.1% TFA)

출처 및 근거

ORD 기록
ord-7de699da68554f92a8a384ee3436799f
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08470841B2

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