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Methanol → Methyl 1-(methylamino)cyclopropanecarboxylate hydrochloride

HRID 2248954
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HRID 2248954 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

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

생성물 1

HCID 19995335Methyl 1-(methylamino)cyclopropanecarboxylate hydrochloride수율 86.6%

실험 절차

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.

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후처리

  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

출처 및 근거

ORD 기록
ord-4c92e9f41b4d4213b43a084e94c35d08
출처 데이터셋
uspto-grants-1991_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05041612

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