Water → HCID 178448115, 화합물

HRID 1663003노트

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HRID 1663003 반응식
[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]

참가 물질

7

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 516892Sodium BicarbonateHCID 178489931HCID 178489931, 화합물

생성물 1

HCID 178448115HCID 178448115, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 6212Chloroform용매

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6e12803540354716b8c7cc8bba4ae9e5
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08034814B2

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