Triethylamine → 4-(4-Nitrophenyl)butyl methanesulfonate

HRID 1375720

反応式

HRID 1375720 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([CH2:10][CH2:11][CH2:12][CH2:13][OH:14])=[CH:6][CH:5]=1)([O-:3])=[O:2].C(N(CC)CC)C.[CH3:22][S:23](Cl)(=[O:25])=[O:24]>C(Cl)Cl>[CH3:22][S:23]([O:14][CH2:13][CH2:12][CH2:11][CH2:10][C:7]1[CH:6]=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:9][CH:8]=1)(=[O:25])=[O:24]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 5908694-Nitrobenzenebutanol

生成物 1

HCID 147295324-(4-Nitrophenyl)butyl methanesulfonate収率 98%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

4-(4-Nitrophenyl)-1-Butanol (2.5 g, 12.166 mmol) was dissolved in DCM (50 ml). The solution was cooled in an ice-bath. Triethylamine (2.45 ml, 15.2 mmol) was added and then methanesulfonyl chloride (1.533 g, 13.382 mmol) was dropped in. After 1 hour, the ice-bath was removed. The mixture was stirred for 4 hours more. The reaction mixture was washed with water, sodium hydrogencarbonate aqueous solution (1%) and water (×3) and dried with magnesium sulfate. The solvent was evaporated in vacuum and the desired product (3.25 g) was obtained, yield 98%.

後処理

  1. temperatureThe solution was cooled in an ice-bath
  2. customthe ice-bath was removed
  3. washThe reaction mixture was washed with water, sodium hydrogencarbonate aqueous solution (1%) and water (×3)
  4. dry with materialdried with magnesium sulfate
  5. customThe solvent was evaporated in vacuum

出典と根拠

ORDレコード
ord-2fb8b0369a2348e2996f5f4b9ff85684
出典データセット
uspto-grants-2007_01
特許番号
US07169810B2

関連ノート

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