Pyridine → Ethyl 2-(((benzyloxy)carbonyl)amino)-2-cyanoacetate

HRID 256598

反応式

HRID 256598 の反応式
[CH2:1]([O:3][C:4](=[O:9])[CH:5]([NH2:8])[C:6]#[N:7])[CH3:2].N1C=CC=CC=1.[CH2:16]([O:23][C:24](Cl)=[O:25])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>O>[CH2:1]([O:3][C:4](=[O:9])[CH:5]([NH:8][C:24]([O:23][CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)=[O:25])[C:6]#[N:7])[CH3:2]

参加物

5

反応物 3

HCID 1049PyridineHCID 10387Benzyl chloroformateHCID 288716Ethyl 2-amino-2-cyanoacetate

生成物 1

HCID 9943163Ethyl 2-(((benzyloxy)carbonyl)amino)-2-cyanoacetate収率 60.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a stirred mixture of 2-amino-2-cyanoacetic acid ethyl ester (19.7 g) and pyridine (12.2 g) in water (123 ml) was added portionwise benzyloxycarbonyl chloride (27.9 g) under ice cooling. The resulting mixture was stirred under ice cooling for 1 hour. Precipitated crystals were collected, washed thoroughly with water, and recrystallized from ethanol to give the title compound (24.2 g, 60.2%) as colorless crystals, mp 111°-112° C.

後処理

  1. customPrecipitated crystals
  2. customwere collected
  3. washwashed thoroughly with water
  4. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-4ea026a1293a48e196c3c781eb05705b
出典データセット
uspto-grants-1993_11
特許番号
US05258382

関連ノート

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