Sodium Methoxide → 2-Piperidinone, 3-amino-3-(difluoromethyl)-

HRID 1903842노트

반응식

HRID 1903842 반응식
C[O:2][C:3](=O)[C:4]([CH:10]([F:12])[F:11])([NH2:9])[CH2:5][CH2:6][CH2:7][NH2:8].C1(N)C(F)=C(F)C(F)=C(N)C=1F.Cl.Cl.C[O-].[Na+]>CO>[NH2:9][C:4]1([CH:10]([F:12])[F:11])[CH2:5][CH2:6][CH2:7][NH:8][C:3]1=[O:2]

참가 물질

4

반응물 2

HCID 10942334Sodium MethoxideHCID 131712630HCID 131712630, 화합물

생성물 1

HCID 5746312-Piperidinone, 3-amino-3-(difluoromethyl)-

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

To a solution of methyl-2-difluoromethyl-2,5-diaminopentanoate-dihydrochloride (2.7 g) in dry methanol (30 ml) is added under nitrogen 2 equivalents of sodium methylate in methanol (0.46 g of sodium in 20 ml of methanol). The reaction mixture is stirred for 3 hours at room temperature then the solvent is evaporated under reduced pressure. The residue is extracted with ether to yield crude 3-amino-3-difluoromethyl-2-piperidone which is purified either by crystallization from CHCl3 /pentane: (m.p.: 149° C.) or by distillation (b.p. 135° C./0.05 mmHg).

후처리

  1. customthe solvent is evaporated under reduced pressure
  2. extractionThe residue is extracted with ether

출처 및 근거

ORD 기록
ord-ea30bd9b47a64303b0a8057e6b1b4da9
출처 데이터셋
uspto-grants-1984_03
특허 번호
US04438270

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