Triethylamine → Ethyl 4-methyl-2-(4-methylbenzoylamino)-3-oxopentanoate

HRID 854615ノート

反応式

HRID 854615 の反応式
Cl.[NH2:2][CH:3]([C:9](=[O:13])[CH:10]([CH3:12])[CH3:11])[C:4]([O:6][CH2:7][CH3:8])=[O:5].[CH3:14][C:15]1[CH:23]=[CH:22][C:18]([C:19](Cl)=[O:20])=[CH:17][CH:16]=1.C(N(CC)CC)C>ClCCl>[CH3:11][CH:10]([CH3:12])[C:9](=[O:13])[CH:3]([NH:2][C:19](=[O:20])[C:18]1[CH:22]=[CH:23][C:15]([CH3:14])=[CH:16][CH:17]=1)[C:4]([O:6][CH2:7][CH3:8])=[O:5]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 134054-Methylbenzoyl ChlorideHCID 57434496Ethyl 2-amino-4-methyl-3-oxopentanoate hydrochloride

生成物 1

HCID 57434497Ethyl 4-methyl-2-(4-methylbenzoylamino)-3-oxopentanoate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

10 g of ethyl 2-amino-4-methyl-3-oxopentanoate hydrochloride and 7.4 g of 4-methylbenzoyl chloride are dissolved in 250 ml of dichloromethane, and 13.3 ml of triethylamine are slowly added dropwise at 0° C. The mixture is stirred at room temperature for one hour and then washed with water, the organic phase is separated off and dried over MgSO4 and the solvent is then removed under reduced pressure. This gives 13 g of ethyl 4-methyl-2-(4-methylbenzoylamino)-3-oxopentanoate as an oil. C16H21NO4 (291.35), MS (ESI)=292 (M+H+).

後処理

  1. washwashed with water
  2. customthe organic phase is separated off
  3. dry with materialdried over MgSO4
  4. customthe solvent is then removed under reduced pressure

出典と根拠

ORDレコード
ord-ee3f77be50a5460287543f160d3c0990
出典データセット
uspto-grants-2007_08
特許番号
US07259177B2

反応ノート

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