Ammonia → HCID 178489931, 화합물

HRID 1663004노트

반응식

HRID 1663004 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.C[CH2:22][O:23][C:24]([CH3:26])=O.[NH3:27]>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]([CH2:4][C:1]3[CH:2]=[N:27][C:24]([O:23][CH3:22])=[CH:26][CH:3]=3)=[N:13][N:12]=2)[CH2:6][CH2:5]1)([CH3:3])[CH3:2]

참가 물질

6

반응물 4

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

생성물 1

HCID 178489931HCID 178489931, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Under N2 atmosphere, in an ampoule 1.8 g (12.7 mMol) of trans 4-isopropyl-cyclohexylamine (preparation see Arzneim. Forsch. 1969, 19, 140) and 700 mg (2.4 mMol) of 1-chloro-4-[6-methoxy-pyridin-3-yl)methyl]phthalazine are heated during 14 h at 140° C. The suspension is dissolved by dilution with EtOAc, 1.5 ml of NH3 solution (25%) and water, and the aqueous phase is removed and extracted twice with EtOAc. The organic phases are washed with water and brine, dried (Na2SO4) and evaporated. Crystallization from EtOAc/hexane 1:1 results in the title compound: M.p. 124-125° C.; FAB-MS: (M+H)+=391; HPLC(Grad20-100) tRet12.4.

후처리

  1. customthe aqueous phase is removed
  2. extractionextracted twice with EtOAc
  3. washThe organic phases are washed with water and brine
  4. dry with materialdried (Na2SO4)
  5. customevaporated
  6. customCrystallization from EtOAc/hexane 1:1

출처 및 근거

ORD 기록
ord-4ceb48b07d4646b3bb1e98cfb54e0d38
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08034814B2

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