Methyl chloroformate → HCID 59166438、化合物

HRID 1174402ノート

反応式

HRID 1174402 の反応式
[NH2:1][CH:2]([CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=1)[C:3]([OH:5])=[O:4].Cl[C:14]([O:16][CH3:17])=[O:15]>O1CCOCC1.[OH-].[Na+]>[CH3:17][O:16][C:14]([NH:1][C@H:2]([C:3]([OH:5])=[O:4])[CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=1)=[O:15]

参加物

5

反応物 2

HCID 6586Methyl chloroformateHCID 42104063-Pyridin-2-yl-L-alanine

生成物 1

HCID 59166438HCID 59166438、化合物収率 65.1%

試薬・触媒・溶媒 2

HCID 14798Sodium Hydroxide溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
60 °C

実験手順

A solution of 2-amino-3-pyridin-2-yl-propionic acid (0.168 g, 1.0 mmol) in 1,4-dioxane (1.0 mL) and 1 N NaOH (3.6 mL) was treated with methyl chloroformate (0.153 mL, 2.0 mmol), stirred at 60° C. for 7 hours, and extracted with dichloromethane. The aqueous phase was acidified to pH 7 with 1 N HCl and evaporated to dryness. The resulting solid was trituated with 3:1 dichloromethane/isopropanol, filtered, and the filtrate was concentrated to yield a yellow solid (0.146 g, 65%) which was used for the next step without further purification.

後処理

  1. extractionextracted with dichloromethane
  2. customevaporated to dryness
  3. filtrationfiltered
  4. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-2313a1cb47404fb789d8e40de042635f
出典データセット
uspto-grants-2010_11
特許番号
US07834043B2

反応ノート

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