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Borane → Butyl[(2,3-dimethoxyphenyl)methyl]amine

HRID 1725241
ノート
印刷プレビュー

反応式

HRID 1725241 の反応式
[CH2:1]([NH:5][C:6](=O)[C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([O:13][CH3:14])[C:8]=1[O:15][CH3:16])[CH2:2][CH2:3][CH3:4].B>C1COCC1.C(OCC)C>[CH2:1]([NH:5][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([O:13][CH3:14])[C:8]=1[O:15][CH3:16])[CH2:2][CH2:3][CH3:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 6331BoraneHCID 347459N-butyl-2,3-dimethoxybenzamide

生成物 1

HCID 4717318Butyl[(2,3-dimethoxyphenyl)methyl]amine収率 54.3%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

N-Butyl-2,3-dimethoxybenzamide (5.37 g, 22.6 mmol) was dissolved in freshly distilled THF (230 mL) and cooled in an ice bath under an argon atmosphere. Borane (28 mL of a 2 M solution of the dimethylsulfide complex in diethyl ether) was added and the ice bath was removed after 15 minutes. The reaction mixture was refluxed overnight and was then allowed to cool to room temperature. The reaction was quenched by careful addition of 10% HCl (11 mL) and the mixture was stirred for four hours and then concentrated in vacuo. The residue was taken up in ethyl acetate (300 mL) and washed with aqueous 2 M K2CO3 (3×100 mL), and brine (100 mL), dried over Na2SO4, and concentrated in vacuo. Purification on silica gel (160 g) with ethyl acetate (33-100% gradient) in heptane and finally 5% ethanol in ethyl acetate as the eluent yielded 2.74 g (54%) of a light yellow oil.

後処理

  1. temperaturecooled in an ice bath under an argon atmosphere
  2. customthe ice bath was removed after 15 minutes
  3. temperatureThe reaction mixture was refluxed overnight
  4. customThe reaction was quenched by careful addition of 10% HCl (11 mL)
  5. concentrationconcentrated in vacuo
  6. washwashed with aqueous 2 M K2CO3 (3×100 mL), and brine (100 mL)
  7. dry with materialdried over Na2SO4
  8. concentrationconcentrated in vacuo
  9. customPurification on silica gel (160 g) with ethyl acetate (33-100% gradient) in heptane and finally 5% ethanol in ethyl acetate as the eluent

出典と根拠

ORDレコード
ord-a3db7ae055174b3597fcde40db085e0d
出典データセット
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07488844B2

反応ノート

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