Methyl chloroformate → HCID 86740383、化合物

HRID 464781

反応式

HRID 464781 の反応式
Cl.[NH2:2][C:3](OCC)=[CH:4][C:5]([O:7][CH2:8][CH3:9])=[O:6].CN1CC[O:17][CH2:16][CH2:15]1.Cl[C:21]([O:23][CH3:24])=[O:22]>C(Cl)Cl>[CH3:24][O:23][C:21](=[O:22])[N:2]=[CH:3][CH2:4][C:5]([O:7][CH2:8][CH2:9][O:17][CH2:16][CH3:15])=[O:6]

参加物

5

反応物 3

HCID 6586Methyl chloroformateHCID 79724-MethylmorpholineHCID 53395434Ethyl beta-amino-beta-ethoxyacrylate hydrochloride

生成物 1

HCID 86740383HCID 86740383、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution consisting of 96 g of ethyl β-amino-β-ethoxyacrylate hydrochloride, 800 ml of methylene chloride and 120 ml of N-methylmorpholine is warmed to 40°. While stirring there is added dropwise within 2 hours a solution of 65 ml of methyl chloroformate in 350 ml of methylene chloride. After completion of the addition, the mixture is stirred at 40° for a further 2 hours. Thereupon, the resulting salt is filtered off under suction and washed with about 50 ml of methylene chloride. The filtrate is evaporated at 40° in a water-jet vacuum. There is obtained crude methyl[(1-ethoxy-2-ethoxycarbonyl)-ethylidene]carbamate in the form of a pale yellow oil which is used immediately in the next step.

後処理

  1. temperatureis warmed to 40°
  2. additionAfter completion of the addition
  3. stirringthe mixture is stirred at 40° for a further 2 hours
  4. filtrationThereupon, the resulting salt is filtered off under suction
  5. washwashed with about 50 ml of methylene chloride
  6. customThe filtrate is evaporated at 40° in a water-jet vacuum

出典と根拠

ORDレコード
ord-9784dfae229a4f8299c9b1e165277e01
出典データセット
uspto-grants-1985_10
特許番号
US04549019

関連ノート

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