Morpholine → 4-[5-(1,1-Dimethoxyethyl)-2-methoxy-3-trifluoromethylphenyl]morpholine

HRID 249725

반응식

HRID 249725 반응식
Br[C:2]1[CH:7]=[C:6]([C:8]([O:12][CH3:13])([O:10][CH3:11])[CH3:9])[CH:5]=[C:4]([C:14]([F:17])([F:16])[F:15])[C:3]=1[O:18][CH3:19].C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1.[NH:66]1[CH2:71][CH2:70][O:69][CH2:68][CH2:67]1>>[CH3:11][O:10][C:8]([C:6]1[CH:5]=[C:4]([C:14]([F:17])([F:16])[F:15])[C:3]([O:18][CH3:19])=[C:2]([N:66]2[CH2:71][CH2:70][O:69][CH2:68][CH2:67]2)[CH:7]=1)([O:12][CH3:13])[CH3:9]

참가 물질

4

반응물 3

HCID 8083MorpholineHCID 634876Binap, (A+-)-HCID 580856971-Bromo-5-(1,1-dimethoxyethyl)-2-methoxy-3-trifluoromethylbenzene

생성물 1

HCID 580856994-[5-(1,1-Dimethoxyethyl)-2-methoxy-3-trifluoromethylphenyl]morpholine

실험 절차

1-Bromo-5-(1,1-dimethoxyethyl)-2-methoxy-3-trifluoromethylbenzene (2 g) was initially introduced and argon was passed through with stirring for 0.5 h. Subsequently, the mixture was treated with Pd(II) acetate (13 mg), BINAP (54 mg) and sodium tertiary-butylate (784 mg), followed by morpholine (0.6 ml). The mixture obtained was stirred under argon at 85° C. for 8 h and after standing overnight at RT it was stirred at 85° C. for a further 8 h and allowed to stand overnight. The solvent was then stripped off and the residue was purified on silica gel (n-heptane-ethyl acetate gradient). 468 mg of the desired product were obtained.

후처리

  1. customThe mixture obtained
  2. stirringwas stirred under argon at 85° C. for 8 h
  3. waitafter standing overnight at RT
  4. stirringit was stirred at 85° C. for a further 8 h
  5. waitto stand overnight
  6. customthe residue was purified on silica gel (n-heptane-ethyl acetate gradient)

출처 및 근거

ORD 기록
ord-60483acf475248b1b8834088ccafcae2
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07863269B2

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