Triethylamine → HCID 18760490、化合物

HRID 1017962ノート

反応式

HRID 1017962 の反応式
C(N(CC)CC)C.[C:8](Cl)(=[O:13])[C:9]([CH3:12])([CH3:11])[CH3:10].[CH2:15]([C:17]1([CH2:27][CH3:28])[C:22](=[O:23])[O:21][CH2:20][C:19]([CH3:26])([CH2:24][OH:25])[NH:18]1)[CH3:16]>CN(C)C1C=CN=CC=1.ClCCl>[CH2:27]([C:17]1([CH2:15][CH3:16])[C:22](=[O:23])[O:21][CH2:20][C:19]([CH3:26])([CH2:24][O:25][C:8](=[O:13])[C:9]([CH3:12])([CH3:11])[CH3:10])[NH:18]1)[CH3:28]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 62493Pivaloyl chlorideHCID 187604863,3-Diethyl-5-methyl-5-hydroxymethylmorpholin-2-one

生成物 1

HCID 18760490HCID 18760490、化合物

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

2.4 ml (0.017 mol) of triethylamine and then 2.15 g 2 (0.018 mol) of pivaloyl chloride are added dropwise to a solution of 3.45 g (0.017 mol) of 3,3-diethyl-5-methyl-5-hydroxymethylmorpholin-2-one and 0.1 g of 4-dimethylaminopyridine in 20 ml dichloromethane at 15° C. After stirring for 20 hours, the precipitated triethylaminehydrochloride is removed by filtration and the filtrate is washed with water, dried over MgSO4 and concentrated by evaporation in a rotary evaporator. The residue is recrystallised from hexane. This gives 3.9 g (77%) of compound (217), m.p. 51-53° C.

後処理

  1. customthe precipitated triethylaminehydrochloride is removed by filtration
  2. washthe filtrate is washed with water
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated by evaporation in a rotary evaporator
  5. customThe residue is recrystallised from hexane

出典と根拠

ORDレコード
ord-51729c83667448aa8204b9620394a9c1
出典データセット
uspto-grants-2002_11
特許番号
US06479608B1

反応ノート

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