Water → HCID 178448115、化合物

HRID 1663003ノート

反応式

HRID 1663003 の反応式
[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]([CH2:21][C:22]3[CH:23]=[N:24][C:25]([O:28]C)=[CH:26][CH:27]=3)=[N:13][N:12]=2)[CH2:6][CH2:5]1)([CH3:3])[CH3:2].C([O-])(O)=O.[Na+].O.CCOC(C)=O>C(Cl)(Cl)Cl.CO>[CH:1]([C@H:4]1[CH2:5][CH2:6][C@H:7]([NH:10][C:11]2[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[C:14]([CH2:21][C:22]3[CH:23]=[N:24][C:25]([OH:28])=[CH:26][CH:27]=3)=[N:13][N:12]=2)[CH2:8][CH2:9]1)([CH3:3])[CH3:2]

参加物

7

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 516892Sodium BicarbonateHCID 178489931HCID 178489931、化合物

生成物 1

HCID 178448115HCID 178448115、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6212Chloroform溶媒

反応条件

温度
60 °C

実験手順

Under N2 atmosphere, 0.35 ml (2.6 mMol) of Me3Sil are added to 500 mg (1.3 mMol) of trans 1-(4-isopropyl-cyclohexylamino)-4-[6-methoxy-(pyridin-3-yl)-methyl]-phthalazine in 15 ml of chloroform, followed by stirring for 16 h at 60° C. After cooling to RT, 15 ml of sat. NaHCO3 solution, 10 ml of water, EtOAc and a small amount of methanol are added, followed by agitation. From the resulting solution, the aqueous phase is removed and extracted twice with EtOAc. The organic phases are washed with water and brine, dried (Na2SO4) and evaporated to dryness. Crystallization by partial evaporation of a solution in methanol results in the title compound: M.p. 271-272° C. (decomposition); FAB-MS: (M+H)+=377; HPLC(Grad20-100) tRet=10.2.

後処理

  1. temperatureAfter cooling to RT
  2. customFrom the resulting solution, the aqueous phase is removed
  3. extractionextracted twice with EtOAc
  4. washThe organic phases are washed with water and brine
  5. dry with materialdried (Na2SO4)
  6. customevaporated to dryness
  7. customCrystallization
  8. customby partial evaporation of a solution in methanol

出典と根拠

ORDレコード
ord-6e12803540354716b8c7cc8bba4ae9e5
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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