Water → 1-(Morpholin-4-ylcarbonyl)-5-[4-(trifluoromethyl)phenyl]piperidine-3-carboxamide

HRID 1642811노트

반응식

HRID 1642811 반응식
C(N(CC)CC)C.[N:8]1([C:14](Cl)=[O:15])[CH2:13][CH2:12][O:11][CH2:10][CH2:9]1.C(O)(=O)C.[F:21][C:22]([F:39])([F:38])[C:23]1[CH:28]=[CH:27][C:26]([CH:29]2[CH2:34][NH:33][CH2:32][CH:31]([C:35]([NH2:37])=[O:36])[CH2:30]2)=[CH:25][CH:24]=1.O>ClCCl>[N:8]1([C:14]([N:33]2[CH2:34][CH:29]([C:26]3[CH:25]=[CH:24][C:23]([C:22]([F:39])([F:38])[F:21])=[CH:28][CH:27]=3)[CH2:30][CH:31]([C:35]([NH2:37])=[O:36])[CH2:32]2)=[O:15])[CH2:13][CH2:12][O:11][CH2:10][CH2:9]1

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 848104-Morpholinecarbonyl chlorideHCID 667551875-[4-(Trifluoromethyl)phenyl]piperidine-3-carboxamide acetate

생성물 1

HCID 580024451-(Morpholin-4-ylcarbonyl)-5-[4-(trifluoromethyl)phenyl]piperidine-3-carboxamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

At 0° C., 0.56 g (5.52 mmol) of triethylamine and 0.55 g (3.70 mmol) of morpholine-4-carbonyl chloride were added to a solution of 0.61 mg (1.85 mmol) of 5-[4-(trifluoromethyl)phenyl]piperidine-3-carboxamide acetate (Example 51A) in 10 ml of dichloromethane. The reaction mixture was stirred at RT for 1 h. After addition of water and phase separation, the organic phase was dried over sodium sulphate, filtered and concentrated under reduced pressure. This gave 0.61 g (100% of theory) of crude product in a purity of 77% (LC-MS), which was reacted without any further purification steps.

후처리

  1. dry with materialthe organic phase was dried over sodium sulphate
  2. filtrationfiltered
  3. concentrationconcentrated under reduced pressure
  4. customThis gave 0.61 g (100% of theory) of crude product in a purity of 77% (LC-MS), which was reacted without any further purification steps

출처 및 근거

ORD 기록
ord-b338b43ebd074d9cb6644ec3b97a0b2e
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08119663B2

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