Ammonia → HCID 178448116、化合物

HRID 747852ノート

反応式

HRID 747852 の反応式
[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]

参加物

6

反応物 4

HCID 222AmmoniaHCID 962WaterHCID 9207Phthalazine2 回HCID 178448118HCID 178448118、化合物

生成物 1

HCID 178448116HCID 178448116、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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.

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-c6f6954f88d54203b5aac40efa587971
出典データセット
uspto-grants-2008_07
特許番号
US07399761B2

反応ノート

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