Diethyl Ether → 2-Ethoxycarbonyl-1,1-dimethylethylisocyanate

HRID 2309680ノート

反応式

HRID 2309680 の反応式
Cl[C:2](OC(Cl)(Cl)Cl)=[O:3].[CH2:9]([O:11][C:12](=[O:18])[CH2:13][C:14]([NH2:17])([CH3:16])[CH3:15])[CH3:10].C(N(CC)CC)C.CCOCC>C(Cl)Cl>[CH2:9]([O:11][C:12]([CH2:13][C:14]([N:17]=[C:2]=[O:3])([CH3:16])[CH3:15])=[O:18])[CH3:10]

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 8471TriethylamineHCID 10426DiphosgeneHCID 11480520Ethyl 3-amino-3-methylbutanoate

生成物 1

HCID 139389532-Ethoxycarbonyl-1,1-dimethylethylisocyanate収率 99%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of trichloromethyl chloroformate (4.1 g) in methylene chloride (15 ml) is slowly added to a stirred mixture of ethyl-3-amino-3-methylbutanoate (3 g), triethylamine (6.6 g) and methylene chloride (30 ml) at 5° C. The mixture is stirred overnight at room temperature, refluxed for 3 hours, cooled and anhydrous ether added thereto. The precipitated triethylamine hydrochloride is filtered and the filtrate evaporated to yield 2-ethoxycarbonyl-1,1-dimethylethylisocyanate as an oil (3.5 g).

後処理

  1. temperaturerefluxed for 3 hours
  2. temperaturecooled
  3. filtrationThe precipitated triethylamine hydrochloride is filtered
  4. customthe filtrate evaporated

出典と根拠

ORDレコード
ord-27d8fd05bfee402ca80ceb4d43829dd6
出典データセット
uspto-grants-1987_09
特許番号
US04696927

反応ノート

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