Hydrochloric Acid → HCID 58711709, 화합물

HRID 2059896노트

반응식

HRID 2059896 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 58711709HCID 58711709, 화합물수율 80%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
25 °C

실험 절차

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%

후처리

  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

출처 및 근거

ORD 기록
ord-d262a7fc0de1485294f3ca51f5eeebd8
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08278319B2

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