Methanol → HCID 67244427、化合物
反応式
[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]=1参加物
4
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-5cd0066e2f6e41dca976b0405a1c06fd
- 出典データセット
- uspto-grants-2011_06
- 特許番号
- US07960584B2
反応ノート
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