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Methanol → Methyl 1-(methylamino)cyclopropanecarboxylate hydrochloride

HRID 2248954
ノート
印刷プレビュー

反応式

HRID 2248954 の反応式
S(Cl)([Cl:3])=O.[CH3:5][NH:6][C:7]1([C:10]([OH:12])=[O:11])[CH2:9][CH2:8]1.[CH3:13]O>>[ClH:3].[CH3:5][NH:6][C:7]1([C:10]([O:12][CH3:13])=[O:11])[CH2:9][CH2:8]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 3861971-(Methylamino)cyclopropane-1-carboxylic acid

生成物 1

HCID 19995335Methyl 1-(methylamino)cyclopropanecarboxylate hydrochloride収率 86.6%

実験手順

86.5 g (1.2 mol) of thionyl chloride were added dropwise to 300 ml of methanol at -10° C., and thereafter 36.9 g (0.32 mol) of 1-methylamino-cyclopropane-1-carboxylic acid were introduced in portions. Stirring was carried out for 5 hours at room temperature, and the mixture was allowed to stand overnight. The mixture was worked up by filtering it, evaporating down the filtrate in vacuo and heating the residue together with 7 g of active carbon for 10 minutes in methanol. After filtration and evaporation, 45.9 g (86.6% of theory) of methyl 1-methylamino-cyclopropane-1-carboxylate hydrochloride were obtained as a yellowish viscous oil of refractive index nD23.5 : 1.4798.

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

後処理

  1. waitto stand overnight
  2. filtrationby filtering it
  3. customevaporating down the filtrate in vacuo
  4. temperatureheating the residue together with 7 g of active carbon for 10 minutes in methanol
  5. filtrationAfter filtration and evaporation

出典と根拠

ORDレコード
ord-4c92e9f41b4d4213b43a084e94c35d08
出典データセット
uspto-grants-1991_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05041612

反応ノート

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