Dichloromethane → 3-(4-Bromophenyl)propyl methanesulphonate

HRID 217784

反応式

HRID 217784 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][CH2:10][OH:11])=[CH:4][CH:3]=1.ClCCl.[CH3:15][S:16](Cl)(=[O:18])=[O:17]>C(N(CC)CC)C>[CH3:15][S:16]([O:11][CH2:10][CH2:9][CH2:8][C:5]1[CH:4]=[CH:3][C:2]([Br:1])=[CH:7][CH:6]=1)(=[O:18])=[O:17]

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 31297Methanesulfonyl chlorideHCID 105606143-(4-Bromophenyl)propan-1-ol

生成物 1

HCID 196884663-(4-Bromophenyl)propyl methanesulphonate収率 91.5%

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

反応条件

温度
0 °C

実験手順

3-(4-Bromophenyl)propan-1-ol (335 g) and dichloromethane (2.5 L) was charged into Reactor 1. Reactor 1 was adjusted to −10 to 0° C. Triethylamine (205 g) was charged into Reactor 1. Methanesulphonyl chloride (272.7 g) was added dropwise into Reactor 1 maintaining contents at <0° C. Reactor 1 was stirred at −5 to 5° C. for 1 h then analysed for reaction completion. The organic layer was washed with water (1 L) and saturated NaCl solution (1 L). The organic layer was evaporated down to dryness to give 3-(4-bromophenyl)propyl methanesulfonate (418 g).

後処理

  1. customReactor 1 was adjusted to −10 to 0° C
  2. customthen analysed for reaction completion
  3. washThe organic layer was washed with water (1 L) and saturated NaCl solution (1 L)
  4. customThe organic layer was evaporated down to dryness

出典と根拠

ORDレコード
ord-7e3f71f2fd514fcd9d7d6fb40e69d52f
出典データセット
uspto-grants-2012_06
特許番号
US08198285B2

関連ノート

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