Hydrochloric Acid → HCID 58711709、化合物

HRID 2059896ノート

反応式

HRID 2059896 の反応式
[F:1][C:2]([F:14])([F:13])[C:3]1[CH:4]=[C:5]([S:9](Cl)(=[O:11])=[O:10])[CH:6]=[CH:7][CH:8]=1.Cl.[NH:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH:17]1[CH2:22][C:23]([O:25][CH3:26])=[O:24].C(N(CC)CC)C.Cl>ClCCl>[F:1][C:2]([F:14])([F:13])[C:3]1[CH:4]=[C:5]([S:9]([N:16]2[CH2:21][CH2:20][CH2:19][CH2:18][CH:17]2[CH2:22][C:23]([O:25][CH3:26])=[O:24])(=[O:11])=[O:10])[CH:6]=[CH:7][CH:8]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 27332503-(Trifluoromethyl)benzenesulfonyl chlorideHCID 13778732Methyl 2-(piperidin-2-yl)acetate hydrochloride

生成物 1

HCID 58711709HCID 58711709、化合物収率 80%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
25 °C

実験手順

A solution of 3-(trifluoromethyl)benzenesulfonyl chloride (1 eq) in dichloromethane (1.6 ml/mmol) was added dropwise to a cooled solution (0° C.) of methyl 2-(piperidin-2-yl)acetate hydrochloride (1.1 eq) in dichloromethane (40 ml/mmol) and triethylamine (2.5 eq). The mixture was stirred for 90 min at 25° C., after which the reaction was completed (thin-layer chromatographic analysis). Hydrogen chloride solution (0.5 mol/l, 2 ml/mmol) was added and the mixture was stirred for 15 min. The organic phase was separated off, washed with water, dried over sodium sulfate and concentrated to small volume under vacuum. Yield: 80%

後処理

  1. stirringthe mixture was stirred for 15 min
  2. customThe organic phase was separated off
  3. washwashed with water
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated to small volume under vacuum

出典と根拠

ORDレコード
ord-d262a7fc0de1485294f3ca51f5eeebd8
出典データセット
uspto-grants-2012_10
特許番号
US08278319B2

反応ノート

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