Water → HCID 86633450, 화합물

HRID 1668657노트

반응식

HRID 1668657 반응식
Cl[C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=2)[N:3]=1.[NH:15]1[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[C:17]([CH2:24][CH2:25][NH2:26])=[CH:16]1.CCN(C(C)C)C(C)C.O>CC(O)C>[Cl:8][C:6]1[N:5]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=2)[N:3]=[C:2]([NH:26][CH2:25][CH2:24][C:17]2[C:18]3[C:23](=[CH:22][CH:21]=[CH:20][CH:19]=3)[NH:15][CH:16]=2)[CH:7]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 1150TryptamineHCID 81531DiisopropylethylamineHCID 120574654,6-dichloro-2-(2-pyridinyl)pyrimidine2회

생성물 1

HCID 86633450HCID 86633450, 화합물

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

4,6-Dichloro-2-pyridin-2-yl-pyrimidine (Intermediate F) (1 eq, 8.85 mmol, 2.0 g) and 2-(1H-indol-3-yl)-ethylamine (1 eq, 8.85 mmol, 1.42 g) are dissolved in iPrOH (10 ml). DIPEA (2 eq, 17.7 mmol, 2.29 g) is added and the resulting mixture is heated using microwave radiation at 130° C. for 20 min. The reaction mixture is added to water and extracted with EtOAc. The combined organic layers are washed with brine, dried (MgSO4), filtered, and concentrated in vacuo. The crude residue is crystallised from EtOAc giving the title compound [M+H]+=350.

후처리

  1. temperaturethe resulting mixture is heated
  2. customat 130° C.
  3. customfor 20 min
  4. extractionextracted with EtOAc
  5. washThe combined organic layers are washed with brine
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customThe crude residue is crystallised from EtOAc giving the title compound [M+H]+=350

출처 및 근거

ORD 기록
ord-31020f863ec64a8aa41a32598dba3fda
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07989458B2

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