Methyl iodide → 4-Iodo-α-(methoxymethyl)benzeneethanamine
반응식
[NH2:1][CH:2]([CH2:5][C:6]1[CH:11]=[CH:10][C:9]([I:12])=[CH:8][CH:7]=1)[CH2:3][OH:4].I[CH3:14]>C1COCC1>[I:12][C:9]1[CH:8]=[CH:7][C:6]([CH2:5][CH:2]([NH2:1])[CH2:3][O:4][CH3:14])=[CH:11][CH:10]=1참가 물질
4
반응 조건
- 온도
- 0 °C
실험 절차
A mixture of 12.0 g (43.3 mmol) 2-amino-3-(4-iodophenyl)-propan-1-ol (I41) and 350 mL THF is cooled down to 0° C. 3.81 g (95 mmol) NAH (60% in min. oil) are carefully added and the mixture is stirred at 0° C. for 30 min. 3.25 mL (52.0 mmol) iodomethane are added and cooling is removed. The reaction mixture is stirred at r.t. for 1 h. The mixture is poured onto water and extracted with EtOAc (2×). The combined organic layers are washed with brine, dried with Na2SO4 and the solvent is removed in vacuo. The compound is used without further purification.
후처리
- addition3.81 g (95 mmol) NAH (60% in min. oil) are carefully added
- temperaturecooling
- customis removed
- stirringThe reaction mixture is stirred at r.t. for 1 h
- additionThe mixture is poured onto water
- extractionextracted with EtOAc (2×)
- washThe combined organic layers are washed with brine
- dry with materialdried with Na2SO4
- customthe solvent is removed in vacuo
- customThe compound is used without further purification
출처 및 근거
- ORD 기록
- ord-3eb18557454a4f82bcb5a98ee192ea61
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08835472B2
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