Triethylamine → N-(2-hydroxy-5-bromophenyl)-3,3-dimethylbutyramide

HRID 48166

반응식

HRID 48166 반응식
[C:1]([CH2:5][C:6](Cl)=[O:7])([CH3:4])([CH3:3])[CH3:2].[NH2:9][C:10]1[CH:15]=[C:14]([Br:16])[CH:13]=[CH:12][C:11]=1[OH:17].C(N(CC)CC)C>C(OCC)C>[OH:17][C:11]1[CH:12]=[CH:13][C:14]([Br:16])=[CH:15][C:10]=1[NH:9][C:6](=[O:7])[CH2:5][C:1]([CH3:4])([CH3:3])[CH3:2]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 815143,3-Dimethylbutanoyl chlorideHCID 3518402-Amino-4-Bromophenol

생성물 1

HCID 22742126N-(2-hydroxy-5-bromophenyl)-3,3-dimethylbutyramide수율 31.5%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

A solution of tert-butylacetyl chloride (2.7 g, 0.020 mol) in diethyl ether (20 ml) was added dropwise to a solution of 2-amino-4bromophenol (3.8 g, 0.020 mol) and triethylamine (2.1 g, 0.020 mol) in diethyl ether (160 ml) and the mixture was stirred at room temperature for 3 hours. The mixture was filtered and the filtrate was evaporated in vacuo. Purification by flash column chromatography on silica gel, eluting initially with ethyl acetate:dichloromethane 1.5:98.5 and then with ethyl acetate:dichloromethane 2.5:97.5, gave N-(2-hydroxy-5-bromophenyl)-3,3-dimethylbutyramide (1.8 g).

후처리

  1. filtrationThe mixture was filtered
  2. customthe filtrate was evaporated in vacuo
  3. customPurification by flash column chromatography on silica gel
  4. washeluting initially with ethyl acetate:dichloromethane 1.5:98.5

출처 및 근거

ORD 기록
ord-a4dae2ba05c94e56acd37a42b6eece85
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06703347B2

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