Ammonia → HCID 178489931、化合物

HRID 1663004ノート

反応式

HRID 1663004 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.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]

参加物

6

反応物 4

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

生成物 1

HCID 178489931HCID 178489931、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4ceb48b07d4646b3bb1e98cfb54e0d38
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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