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Acetonitrile → 5-Azaspiro[2.4]heptan-4-one, 7-amino-7-methyl-

HRID 1675192
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인쇄 미리보기

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HRID 1675192 반응식
C(#N)C.Cl.Cl.[NH2:6][C:7]([C:11]1([C:14]([OH:16])=O)[CH2:13][CH2:12]1)([CH3:10])[CH2:8][NH2:9].C[Si](C)(C)N[Si](C)(C)C>CO>[NH2:6][C:7]1([CH3:10])[C:11]2([CH2:13][CH2:12]2)[C:14](=[O:16])[NH:9][CH2:8]1
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참가 물질

5

반응물 3

HCID 6342AcetonitrileHCID 13838HexamethyldisilazaneHCID 574343681-(1,2-Diamino-1-methylethyl)-1-cyclopropanecarboxylate dihydrochloride

생성물 1

HCID 552821195-Azaspiro[2.4]heptan-4-one, 7-amino-7-methyl-

시약·촉매·용매 1

HCID 887Methanol용매

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온도
100 °C

실험 절차

To an acetonitrile solution (70 mL) of the crude product (800 mg, 3.46 mmol) of 1-(1,2-diamino-1-methylethyl)-1-cyclopropanecarboxylate dihydrochloride was added 1,1,1,3,3,3-hexamethyldisilazane (7.38 mL, 34.6 mmol), and the mixture was heated under reflux under a nitrogen atmosphere in an oil bath at 100° C. for 4 hours. Then the solution was cooled to room temperature, and to the solution was added methanol (70 mL). After that, the solvent was removed under reduced pressure. Thus a crude product of 7-amino-7-methyl-5-azaspiro[2.4]heptan-4-one was obtained as a light brown gum-like solid.

후처리

  1. temperaturethe mixture was heated
  2. temperatureThen the solution was cooled to room temperature
  3. customAfter that, the solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-3486e2102cc74134a5816f19c1149860
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08003666B2

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