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

HRID 48166

反応式

HRID 48166 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-a4dae2ba05c94e56acd37a42b6eece85
出典データセット
uspto-grants-2004_03
特許番号
US06703347B2

関連ノート

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