Methanol → HCID 67244427, 화합물
반응식
[NH2:1][C:2]1[C:9]([I:10])=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1Cl.[CH3:12]O>C1COCC1>[NH2:7][CH2:6][C:5]1[CH:4]=[C:3]([CH3:12])[C:2]([NH2:1])=[C:9]([I:10])[CH:8]=1참가 물질
4
실험 절차
4-Amino-3-chloro-5-iodobenzonitrile (65.2 mg, 0.23 mmol) was dissolved in THF at 0° C. After Borane-THF complex (4 eq, 0.94 mmol, 0.94 ml) was slowly added into the reaction mixture. The reaction temperature was heated to reflux. The reaction mixture was stirred for 12 hrs with reflux. After confirming the completion of the reaction, MeOH was added. The mixture was stirred for 4 hrs. The reaction solvent was removed in vacuo. A residue was extracted with Ethyl acetate, washed with H2O and brine, dried with Na2SO4 and concentrated in vacuo to yield 4-Aminomethyl-2-iodo-6-methyl-phenylamine (19.4 mg).
후처리
- additionAfter Borane-THF complex (4 eq, 0.94 mmol, 0.94 ml) was slowly added into the reaction mixture
- temperatureThe reaction temperature was heated to reflux
- temperaturewith reflux
- additionwas added
- stirringThe mixture was stirred for 4 hrs
- customThe reaction solvent was removed in vacuo
- extractionA residue was extracted with Ethyl acetate
- washwashed with H2O and brine
- dry with materialdried with Na2SO4
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-5cd0066e2f6e41dca976b0405a1c06fd
- 출처 데이터셋
- uspto-grants-2011_06
- 특허 번호
- US07960584B2
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