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

HRID 41703노트

반응식

HRID 41703 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-912b160d0d294e57b5d2e395040ec0ab
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08530657B2

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