Sodium Bicarbonate → Ethyl N-(2,3-dimethyl-2-isopropyl-1-oxobutyl)glycinate

HRID 904102ノート

反応式

HRID 904102 の反応式
C(=O)(O)[O-].[Na+].Cl.[CH2:7]([O:9][C:10](=[O:13])[CH2:11][NH2:12])[CH3:8].[CH3:14][C:15]([CH:22]([CH3:24])[CH3:23])([CH:19]([CH3:21])[CH3:20])[C:16](Cl)=[O:17]>O.CCOCC>[CH2:7]([O:9][C:10](=[O:13])[CH2:11][NH:12][C:16](=[O:17])[C:15]([CH3:14])([CH:22]([CH3:24])[CH3:23])[CH:19]([CH3:21])[CH3:20])[CH3:8]

参加物

6

反応物 3

HCID 516892Sodium BicarbonateHCID 2723640Glycine ethyl ester, hydrochlorideHCID 30166072,3-Dimethyl-2-isopropylbutyryl chloride

生成物 1

HCID 6452343Ethyl N-(2,3-dimethyl-2-isopropyl-1-oxobutyl)glycinate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒

実験手順

Sodium bicarbonate (1.7 g, 0.02 mole) and glycine ethyl ester hydrochloride (1.4 g, 0.01 mole) were dissolved in water (10 ml) and a solution of 2,3-dimethyl-2-isopropylbutanoyl chloride (1.6 g, 0.009 mole) in ether (10 ml) was added. The mixture was stirred vigorously at room temperature for 2 hours. After 16 hours at room temperature the ether layer was separated and dried (MgSO4). Removal of the solvent left a white solid which was recrystallized from ether/petroleum ether to give N-(2,3-dimethyl-2-isopropylbutanoyl)glycine ethyl ester, mp. 74.5°-75.5°.

後処理

  1. customAfter 16 hours at room temperature the ether layer was separated
  2. dry with materialdried (MgSO4)
  3. customRemoval of the solvent
  4. waitleft a white solid which
  5. customwas recrystallized from ether/petroleum ether

出典と根拠

ORDレコード
ord-e93177eb5e544cb6a41c674116fb4662
出典データセット
uspto-grants-1980_10
特許番号
US04230688

反応ノート

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