Ammonia → HCID 178489122, 화합물

HRID 1662998노트

반응식

HRID 1662998 반응식
[CH:1]([C@H:4]1[CH2:9][CH2:8][C@H:7]([NH2:10])[CH2:6][CH2:5]1)([CH3:3])[CH3:2].[CH:11]1[C:20]2[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH:14]=[N:13][N:12]=1.[NH3:21].O.C[CH2:24][O:25][C:26]([CH3:28])=O>>[CH:1]([C@H:4]1[CH2:9][CH2:8][C@H:7]([NH:10][C:11]2[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[C:14]([CH2:5][C:4]3[CH:1]=[CH:2][N:21]=[C:26]([O:25][CH3:24])[CH:28]=3)=[N:13][N:12]=2)[CH2:6][CH2:5]1)([CH3:3])[CH3:2]

참가 물질

6

반응물 5

HCID 222AmmoniaHCID 962WaterHCID 8857Ethyl AcetateHCID 9207PhthalazineHCID 178448118HCID 178448118, 화합물

생성물 1

HCID 178489122HCID 178489122, 화합물

실험 절차

Under N2 atmosphere, in an ampoule 1.73 g (12 mMol) of trans 4-isopropyl-cyclohexylamine (preparation see Arzneim. Forsch. 1969, 19, 140) and 700 mg (2.4 mMol) of 1-chloro-4-[2-methoxy-pyridin-4-yl)methyl]phthalazine are heated during 17 h at 140° C. The reaction mixture is suspended in EtOAc, and 1.5 ml of NH3 solution (25%) and water are added. The isolated aqueous phase is extracted another two times with EtOAc, and the organic phases are washed with water and brine, dried (Na2SO4) and evaporated to dryness. Column chromatography (SiO2; hexane/EtOAc 1:1) results in the title compound: M.p. 65-66° C.; FAB-MS: (M+H)+=391.

후처리

  1. extractionThe isolated aqueous phase is extracted another two times with EtOAc
  2. washthe organic phases are washed with water and brine
  3. dry with materialdried (Na2SO4)
  4. customevaporated to dryness

출처 및 근거

ORD 기록
ord-5425380acb1a4232854225d6491ca12b
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08034814B2

반응 노트

불러오는 중…