Methanol → 4-Cyclopropylpyridin-3-amine
반응식
[Cl-].[NH4+].[CH:3]1([C:6]2[CH:11]=[CH:10][N:9]=[CH:8][C:7]=2[N+:12]([O-])=O)[CH2:5][CH2:4]1.CO>C1COCC1.C(Cl)(Cl)Cl.[Zn]>[CH:3]1([C:6]2[CH:11]=[CH:10][N:9]=[CH:8][C:7]=2[NH2:12])[CH2:5][CH2:4]1참가 물질
7
실험 절차
Zinc powder (223.2 mg, 3.41 mmol) and ammonium chloride solution (365 mg, 6.8 mmol) were added to a stirred solution of 4-cyclopropyl-3-nitropyridine (I-1a: 70 mg, 0.426 mmol) in dry THF (2 mL) at 0° C. and the resulting mixture was stirred at room temperature for 1 hour. The reaction was monitored by TLC (10% methanol in CHCl3). The reaction mixture was filtered over celite bed and washed with THF and filtrate was concentrated. The residue was dissolved in ethyl acetate and washed with water and saturated brine and dried over sodium sulphate and concentrated to afford 450 mg of the product (100% yield).
후처리
- filtrationThe reaction mixture was filtered over celite bed
- washwashed with THF and filtrate
- concentrationwas concentrated
- dissolutionThe residue was dissolved in ethyl acetate
- washwashed with water and saturated brine
- dry with materialdried over sodium sulphate
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-efe3770be40548cdb07366c69f568db4
- 출처 데이터셋
- uspto-grants-2015_05
- 특허 번호
- US09029399B2
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