Sodium Bicarbonate → Ethyl N-((5-methyl-2-(isopropyl)cyclohexyl)carbonyl)glycinate

HRID 903309ノート

反応式

HRID 903309 の反応式
C(=O)(O)[O-].[Na+].Cl.[CH2:7]([O:9][C:10](=[O:13])[CH2:11][NH2:12])[CH3:8].[CH:14]1([CH3:26])[CH2:19][CH2:18][CH:17]([CH:20]([CH3:22])[CH3:21])[CH:16]([C:23](Cl)=[O:24])[CH2:15]1>O.CCOCC>[CH2:7]([O:9][C:10](=[O:13])[CH2:11][NH:12][C:23]([CH:16]1[CH:17]([CH:20]([CH3:22])[CH3:21])[CH2:18][CH2:19][CH:14]([CH3:26])[CH2:15]1)=[O:24])[CH3:8]

参加物

6

反応物 3

HCID 516892Sodium BicarbonateHCID 2723640Glycine ethyl ester, hydrochlorideHCID 13734319Cyclohexanecarbonyl chloride, 5-methyl-2-(1-methylethyl)-

生成物 1

HCID 11521869Ethyl N-((5-methyl-2-(isopropyl)cyclohexyl)carbonyl)glycinate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒

実験手順

Sodium bicarbonate (8.4 g., 0.1 mole) and glycine ethyl ester hydrochloride (7 g. 0.05 mole) were dissolved in water (100 ml.), and a solution of p-menth-3-oyl chloride (10 g., 0.05 mole) in ether (50 ml.) was added and the mixture stirred vigorously at room temperature for 2 hours. At the end of this time the other layer was separated and dried (MgSO4). Removal of the solvent left an oily solid (12.3 g.) This was distilled under reduced pressure to yield N-p-menth-3-oylglycine ethyl ester, bp. 150°-2°/0.1 mm. as a colourless liquid which rapidly solidified.

後処理

  1. customAt the end of this time the other layer was separated
  2. dry with materialdried (MgSO4)
  3. customRemoval of the solvent
  4. waitleft an oily solid (12.3 g.)
  5. distillationThis was distilled under reduced pressure

出典と根拠

ORDレコード
ord-dfefc25f2562433f8e14859e6370921a
出典データセット
uspto-grants-1980_10
特許番号
US04226988

反応ノート

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