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Toluene → 2-(3-Bromophenyl)-2-methylbutan-1-amine

HRID 384088
ノート
印刷プレビュー

反応式

HRID 384088 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([C:8]([CH3:13])([CH2:11][CH3:12])[C:9]#[N:10])[CH:5]=[CH:6][CH:7]=1.[AlH3].C1(C)C=CC=CC=1>C1COCC1>[Br:1][C:2]1[CH:3]=[C:4]([C:8]([CH3:13])([CH2:11][CH3:12])[CH2:9][NH2:10])[CH:5]=[CH:6][CH:7]=1
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 3

HCID 1140TolueneHCID 14488Aluminum hydrideHCID 579696322-(3-Bromophenyl)-2-methylbutanenitrile

生成物 1

HCID 579697762-(3-Bromophenyl)-2-methylbutan-1-amine収率 67%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 2-(3-bromophenyl)-2-methylbutanenitrile (1678.5 mg, 7.049 mmol) in dry THF (28 mL) was cooled in an ice-bath. AlH3:(Me)2EtN complex, 0.5M in PhMe (28.20 mL of 0.5 M, 14.10 mmol) was added slowly dropwise and the resultant solution stirred at 0° C. for 30 mins. The mixture was allowed to warm to RT and stirred for 4.5 hours. The reaction was carefully quenched by dropwise addition of 1:1 THF:water (˜30 mL). The resulting suspension was stirred vigorously and filtered through a pad of celite. The collected solid was partitioned between EtOAc and brine and the aqueous layer further extracted with EtOAc (3×50 mL) and the combined organics dried over Na2SO4, filtered and concentrated under reduced pressure to give a light brown oil. The residue was purified on silica gel by flash column chromatography (5% MeOH in DCM, loaded in DCM, ˜200 mL silica) to give the product as a yellow oil (1137.8 mg, 67% Yield).

後処理

  1. customThe reaction was carefully quenched by dropwise addition of 1:1 THF
  2. stirringThe resulting suspension was stirred vigorously
  3. filtrationfiltered through a pad of celite
  4. customThe collected solid was partitioned between EtOAc and brine
  5. extractionthe aqueous layer further extracted with EtOAc (3×50 mL)
  6. dry with materialthe combined organics dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customto give a light brown oil
  10. customThe residue was purified on silica gel by flash column chromatography (5% MeOH in DCM, loaded in DCM, ˜200 mL silica)

出典と根拠

ORDレコード
ord-a15b2c595b2c48a9ac089bc52ccc0294
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367697B2

反応ノート

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