聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → HCID 178448115，化合物

HRID 1663003笔记

反应方程式

HRID 1663003 反应方程式
[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]

参与物

7

反应物 4

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 8857乙酸乙酯HCID 516892碳酸氢钠HCID 178489931HCID 178489931，化合物

产物 1

HCID 178448115HCID 178448115，化合物

试剂、催化剂与溶剂 2

HCID 887Methanol溶剂HCID 6212三氯甲烷溶剂

反应条件

温度
60 °C

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-6e12803540354716b8c7cc8bba4ae9e5
来源数据集
uspto-grants-2011_10
专利号
US08034814B2

反应笔记

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