Water → HCID 57555222, 화합물

HRID 220816노트

반응식

HRID 220816 반응식
C(=O)([O-])[O-].[K+].[K+].I[CH3:8].[CH:9]1([NH:15][C:16]2[C:17]([NH2:22])=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1.O>CN(C=O)C>[CH:9]1([NH:15][C:16]2[C:17]([NH:22][CH3:8])=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 1517328N-(2-aminophenyl)-N-cyclohexylamine

생성물 1

HCID 57555222HCID 57555222, 화합물수율 39%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Potassium carbonate (2.45 g, 17.7 mmol) and iodomethane (0.81 ml, 13.0 mmol) were added to a solution of N-cyclohexyl-benzene-1,2-diamine from Example E26.2 (2.25 g, 11.8 mmol) in DMF (10 ml). The mixture was stirred for 6 h at room temperature then poured into water and extracted with EtOAc. The organic layer was washed with water then brine, dried and concentrated in vacuo. The residue was purified by flash chromatography on silica gel (eluant; 5% EtOAc:95% hexane) to yield the title compound (950 mg, 39%).

후처리

  1. extractionextracted with EtOAc
  2. washThe organic layer was washed with water
  3. dry with materialbrine, dried
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by flash chromatography on silica gel (eluant; 5% EtOAc:95% hexane)

출처 및 근거

ORD 기록
ord-c29c950c60ad4e6287372633c148642e
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08202858B2

반응 노트

불러오는 중…