Ammonia → HCID 178489122、化合物

HRID 1662998ノート

反応式

HRID 1662998 の反応式
[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]

参加物

6

反応物 5

HCID 222AmmoniaHCID 962WaterHCID 8857Ethyl AcetateHCID 9207PhthalazineHCID 178448118HCID 178448118、化合物

生成物 1

HCID 178489122HCID 178489122、化合物

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5425380acb1a4232854225d6491ca12b
出典データセット
uspto-grants-2011_10
特許番号
US08034814B2

反応ノート

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