Cyanogen Bromide → HCID 86656706, 화합물

HRID 451436노트

반응식

HRID 451436 반응식
Cl.[CH2:2]([C:9]1[CH:14]=[C:13]([CH3:15])[N:12]=[C:11]([NH:16][CH:17]2[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]2)[N:10]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C(=O)([O-])O.[Na+].[C:28](Br)#[N:29]>C(Cl)Cl.O>[CH2:2]([C:9]1[CH:14]=[C:13]([CH3:15])[N:12]=[C:11]([NH:16][CH:17]2[CH2:22][CH2:21][N:20]([C:28]#[N:29])[CH2:19][CH2:18]2)[N:10]=1)[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1

참가 물질

6

반응물 3

HCID 10476Cyanogen BromideHCID 516892Sodium BicarbonateHCID 67344140(4-Benzyl-6-methyl-pyrimidin-2-yl)-piperidin-4-yl-amine hydrochloride

생성물 1

HCID 86656706HCID 86656706, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매3회

반응 조건

온도
0 °C

실험 절차

To a solution of (4-benzyl-6-methyl-pyrimidin-2-yl)-piperidin-4-yl-amine hydrochloride (255 mg, 0.8 mmol) in CH2Cl2 (1.5 mL) was added at 0° C. a suspension of sodium hydrogencarbonate (202 mg, 2.49 mmol) in water (0.5 mL) and then within 1 minute a solution of bromocyan (106 mg, 0.97 mmol) in CH2Cl2 (1 mL). The reaction was stirred at 0° C. for 45 minutes and then at room temperature over night. The reaction was diluted with CH2Cl2, washed with saturated aqueous NaHCO3 solution and with saturated aqueous NaCl solution, dried over sodium sulfate, filtered and the solvent was evaporated under reduced pressure. The residue was purified by column chromatography using a gradient from CH2Cl2 to CH2Cl2/MeOH 19:1 (v/v) as eluent. The title compound was obtained as a colorless oil (135 mg, 55%).

후처리

  1. waitat room temperature over night
  2. washwashed with saturated aqueous NaHCO3 solution and with saturated aqueous NaCl solution
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customthe solvent was evaporated under reduced pressure
  6. customThe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-ab132d7836484e4eb606e6248e0d396d
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486967B2

반응 노트

불러오는 중…