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

HRID 1642811ノート

反応式

HRID 1642811 の反応式
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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b338b43ebd074d9cb6644ec3b97a0b2e
出典データセット
uspto-grants-2012_02
特許番号
US08119663B2

反応ノート

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