Ammonia → HCID 178448116, 화합물

HRID 747852노트

반응식

HRID 747852 반응식
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[N:3][N:2]=1.[CH:11]([C@H:14]1[CH2:19][CH2:18][C@H:17]([NH2:20])[CH2:16][CH2:15]1)([CH3:13])[CH3:12].[NH3:21].[OH2:22]>CCOC(C)=O>[CH:11]([C@H:14]1[CH2:19][CH2:18][C@H:17]([NH:20][C:1]2[C:10]3[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=3)[C:4]([CH2:4][C:5]3[CH:10]=[CH:9][N:21]=[C:7]([OH:22])[CH:6]=3)=[N:3][N:2]=2)[CH2:16][CH2:15]1)([CH3:13])[CH3:12]

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 962WaterHCID 9207Phthalazine2회HCID 178448118HCID 178448118, 화합물

생성물 1

HCID 178448116HCID 178448116, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

trans 1-(4-isoproryl-cyclohexylamino)-4-[2-methoxy-pyridin-4-yl)-methyl]-phthalazine: 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-c6f6954f88d54203b5aac40efa587971
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07399761B2

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