Triethylamine → HCID 68872277、化合物

HRID 2112038ノート

反応式

HRID 2112038 の反応式
[CH2:1]([NH:7][CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].C(N(CC)CC)C.[Br:22][CH2:23][C:24](Cl)=[O:25]>C(Cl)Cl>[CH2:8]([N:7]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6])[C:24](=[O:25])[CH2:23][Br:22])[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 89602Bromoacetyl chlorideHCID 485395Benzenemethanamine, N-hexyl-

生成物 1

HCID 68872277HCID 68872277、化合物収率 58.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

N-hexylbenzylamine (4.2 g, 21.953 mmol) and triethylamine (3.98 ml, 28.539 mmol) were mixed in DCM (20 ml) and cooled in an ice-bath. Bromacetyl chloride (3.455 mg, 21.953 mmol) in DCM (5 ml) was added. The mixture was stirred over weekend and the temperature was allowed going up to room temperature. The mixture was washed with water mixed with 1% hydrochloric acid (water phase pH˜4-5) and brine, dried with magnesium sulphate, and evaporated. Column chromatography of the residue on silica gel using ethyl acetate/heptane (10:90, then 20:80) as eluant gave 4.0 g desired product, yield 58%.

後処理

  1. temperaturecooled in an ice-bath
  2. customwas allowed going up to room temperature
  3. washThe mixture was washed with water
  4. additionmixed with 1% hydrochloric acid (water phase pH˜4-5) and brine
  5. dry with materialdried with magnesium sulphate
  6. customevaporated

出典と根拠

ORDレコード
ord-4a770f917d7d410eaca8f49ddbd503ae
出典データセット
uspto-grants-2009_04
特許番号
US07521461B2

反応ノート

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