Triethylamine → 4-(4-Bromophenyl)-1-(methanesulphonyl)piperidin-4-ol

HRID 41703ノート

反応式

HRID 41703 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([OH:14])[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1.C(N(CC)CC)C.[CH3:22][S:23](Cl)(=[O:25])=[O:24]>ClCCl>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([OH:14])[CH2:9][CH2:10][N:11]([S:23]([CH3:22])(=[O:25])=[O:24])[CH2:12][CH2:13]2)=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 939114-(4-Bromophenyl)-4-hydroxypiperidine

生成物 1

HCID 187232054-(4-Bromophenyl)-1-(methanesulphonyl)piperidin-4-ol

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1 g of 4-(4-bromophenyl)piperidin-4-ol is placed in 20 ml of dichloromethane. 0.65 ml of triethylamine and then 0.33 ml of methanesulphonyl chloride are added. The reaction mixture is stirred at ambient temperature for 2 h. It is washed with water and then with a saturated aqueous sodium chloride solution. The organic phase is dried over sodium sulphate and then evaporated under reduced pressure. The crude product obtained is chromatographed on silica gel, elution being carried out with a dichloromethane/methanol (99/1) solvent mixture. 1.1 g of 4-(4-bromophenyl)-1-(methanesulphonyl)piperidin-4-ol are obtained.

後処理

  1. washIt is washed with water
  2. dry with materialThe organic phase is dried over sodium sulphate
  3. customevaporated under reduced pressure
  4. customThe crude product obtained
  5. customis chromatographed on silica gel, elution

出典と根拠

ORDレコード
ord-912b160d0d294e57b5d2e395040ec0ab
出典データセット
uspto-grants-2013_09
特許番号
US08530657B2

反応ノート

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