Acetyl chloride → HCID 45082407、化合物

HRID 62573ノート

反応式

HRID 62573 の反応式
Cl.[CH3:2][O:3][C:4](=[O:9])[C@@H:5]([CH2:7][OH:8])[NH2:6].C(N(CC)CC)C.[C:17](Cl)(=[O:19])[CH3:18]>ClCCl>[CH3:2][O:3][C:4](=[O:9])[C@@H:5]([CH2:7][OH:8])[NH:6][C:17](=[O:19])[CH3:18]

参加物

5

反応物 3

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 11446470D-Serine methyl ester hydrochloride

生成物 1

HCID 45082407HCID 45082407、化合物収率 90%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
-10 °C

実験手順

D-Serine methyl ester hydrochloride (100 g, 0.6430 mole) was suspended in 500 ml dichloromethane. To this was added triethylamine (136.6 g, 1.35 mole) at 0-5° C., followed by acetyl chloride (53.06 g, 0.6751 mole) drop wise at −10° C. The reaction mixture was stirred at −10° C. for 3 hours, filtered to remove salts and the filtrate was evaporated. The resulting residue was suspended in 400 ml ethyl acetate and stirred for one hour. Salts were filtered and the ethyl acetate layer was concentrated under reduced pressure to get N-acetyl D-serine methyl ester as an oil (93.22 g, Yield: 90%, HPLC: 98.7%),

後処理

  1. filtrationfiltered
  2. customto remove salts
  3. customthe filtrate was evaporated
  4. stirringstirred for one hour
  5. filtrationSalts were filtered
  6. concentrationthe ethyl acetate layer was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-ddb273fd859244429737029322cc5be1
出典データセット
uspto-grants-2016_09
特許番号
US09447024B1

反応ノート

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