Acetonitrile → HCID 12004101, 화합물

HRID 971258노트

반응식

HRID 971258 반응식
Cl[C:2]1[C:3]2[CH2:11][CH2:10][N:9]([C:12]3[C:17]([Cl:18])=[CH:16][CH:15]=[CH:14][N:13]=3)[CH2:8][C:4]=2[N:5]=[CH:6][N:7]=1.[NH2:19][C:20]1[CH:28]=[C:27]2[C:23]([C:24]([CH3:33])([CH3:32])[CH2:25][N:26]2[C:29](=[O:31])[CH3:30])=[CH:22][CH:21]=1.C(#N)C.C(=O)(O)[O-].[Na+]>CCOC(C)=O>[Cl:18][C:17]1[C:12]([N:9]2[CH2:10][CH2:11][C:3]3[C:2]([NH:19][C:20]4[CH:28]=[C:27]5[C:23]([C:24]([CH3:33])([CH3:32])[CH2:25][N:26]5[C:29](=[O:31])[CH3:30])=[CH:22][CH:21]=4)=[N:7][CH:6]=[N:5][C:4]=3[CH2:8]2)=[N:13][CH:14]=[CH:15][CH:16]=1

참가 물질

6

반응물 4

HCID 6342AcetonitrileHCID 516892Sodium BicarbonateHCID 218651761-(6-Amino-3,3-dimethylindolin-1-yl)ethanoneHCID 590214784-Chloro-7-(3-chloropyridin-2-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidine

생성물 1

HCID 12004101HCID 12004101, 화합물수율 79.6%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
180 °C

실험 절차

A mixture of 4-chloro-7-(3-chloropyridin-2-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidine (40 mg, 0.14 mmol), 1-(6-amino-3,3-dimethylindolin-1-yl)ethanone (60 mg, 0.29 mmol), and acetonitrile (3 mL) was heated in a sealed tube via microwave at 180° C. for 60 min. The mixture was treated with EtOAc (50 mL) and saturated aqueous sodium bicarbonate. The organic layer was separated and washed with brine, dried (Na2SO4), and evaporated. The residue was purified by flash chromatography over silica gel to give an off-white solid (50 mg).

후처리

  1. customThe organic layer was separated
  2. washwashed with brine
  3. dry with materialdried (Na2SO4)
  4. customevaporated
  5. customThe residue was purified by flash chromatography over silica gel

출처 및 근거

ORD 기록
ord-412e5b5c6c0e4f23b1cad564a8d9fc7b
출처 데이터셋
uspto-grants-2007_12
특허 번호
US07312330B2

반응 노트

불러오는 중…