Hydrochloric Acid → 4-(Azetidin-3-yl)morpholine dihydrochloride

HRID 377028노트

반응식

HRID 377028 반응식
C1(C(C2C=CC=CC=2)[N:8]2[CH2:11][CH:10]([N:12]3[CH2:17][CH2:16][O:15][CH2:14][CH2:13]3)[CH2:9]2)C=CC=CC=1.[ClH:24]>[OH-].[Pd+2].[OH-].C(O)C>[ClH:24].[ClH:24].[O:15]1[CH2:16][CH2:17][N:12]([CH:10]2[CH2:11][NH:8][CH2:9]2)[CH2:13][CH2:14]1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 211837864-[1-(Diphenylmethyl)azetidin-3-yl]morpholine

생성물 1

HCID 220613264-(Azetidin-3-yl)morpholine dihydrochloride

시약·촉매·용매 2

HCID 9942167Palladium hydroxide촉매HCID 702Ethanol용매

실험 절차

A mixture of 1-diphenylmethyl-3-morpholinoazetidine (Preparation 1(c)) (18.6 g, 60.4 mmol), palladium hydroxide (2 g), ethanol (200 ml) and 1N aqueous HCl (52 ml) was stirred under an atmosphere of hydrogen at 345 kPa (50 p.s.i.) for 3 days. The catalyst was then removed by filtration and the filtrate evaporated to dryness. Addition of dichloromethane (100 ml) to the residue and trituration gave a solid which was recrystallised from methanol to give the title compound (10.2 g) as a crystalline solid. LRMS m/z=179 (m+1)+.

후처리

  1. customThe catalyst was then removed by filtration
  2. customthe filtrate evaporated to dryness
  3. additionAddition of dichloromethane (100 ml) to the residue and trituration
  4. customgave a solid which
  5. customwas recrystallised from methanol

출처 및 근거

ORD 기록
ord-794ca746e92046b0a5488b66bb506bc5
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06022971

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