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Chloroacetic Acid → HCID 43700001、化合物

HRID 2062078
ノート
印刷プレビュー

反応式

HRID 2062078 の反応式
[Cl:1][CH2:2][C:3](O)=[O:4].[CH3:6][O:7][C:8](=[O:13])[C:9]([NH2:12])([CH3:11])[CH3:10].C(N(CC)C(C)C)(C)C>C1COCC1>[CH3:6][O:7][C:8](=[O:13])[C:9]([NH:12][C:3](=[O:4])[CH2:2][Cl:1])([CH3:11])[CH3:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 300Chloroacetic AcidHCID 81531DiisopropylethylamineHCID 4186341Methyl 2-amino-2-methylpropanoate

生成物 1

HCID 43700001HCID 43700001、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 0.95 g chloro acetic acid in 20 ml of dry THF 1.78 g N,N′-carbonyl-diimidazole were added. After 0.5 h at room temperature and under argon atmosphere 1.69 g 2-amino-2-methyl-propionic acid methyl ester and 1.29 g N,N-diisopropyl-ethyl-amine were added and it was stirred for 3 h. Then the solvent was evaporated, the residue taken up in ethyl acetate and washed with 2 M hydrochloric acid, water and sat. aqueous sodium hydrogen carbonate solution. The combined organic fractions were dried over sodium sulphate, filtrated and concentrated. The resulting residue was crystallized from diethylether to yield 2-(2-chloro-acetylamino)-2-methyl-propionic acid methyl ester.

後処理

  1. customThen the solvent was evaporated
  2. washwashed with 2 M hydrochloric acid, water and sat. aqueous sodium hydrogen carbonate solution
  3. dry with materialThe combined organic fractions were dried over sodium sulphate
  4. filtrationfiltrated
  5. concentrationconcentrated
  6. customThe resulting residue was crystallized from diethylether

出典と根拠

ORDレコード
ord-aaffaad8fc7f4287a35f12dfdfab8013
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08283479B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート