Ammonia → HCID 15055868、化合物

HRID 1651561

反応式

HRID 1651561 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][N:23]=2)[O:9][CH:10]2[CH2:15][CH2:14][N:13]([CH2:16][CH2:17][CH2:18][C:19]([OH:21])=O)[CH2:12][CH2:11]2)=[CH:4][CH:3]=1.C1([N:34]=C=NC2CCCCC2)CCCCC1.N>ClCCl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][N:23]=2)[O:9][CH:10]2[CH2:15][CH2:14][N:13]([CH2:16][CH2:17][CH2:18][C:19]([NH2:34])=[O:21])[CH2:12][CH2:11]2)=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 222AmmoniaHCID 23504-((4-Chlorophenyl)-2-pyridinylmethoxy)-1-piperidinebutanoic AcidHCID 10868Dicyclohexylcarbodiimide

生成物 1

HCID 15055868HCID 15055868、化合物収率 76%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

0.50 g (1.29 mmol) of 4-[4-[(4-chlorophenyl)-2-pyridylmethoxy]-1-piperidyl]butanoic acid obtained in Example 28 was dissolved in 5 ml of dichloromethane, and 0.32 g (1.55 mmol) of dicyclohexylcarbodiimide was added to the reaction mixture on an ice bath. Then, 10 ml of ammonia gas dissolved dichloromethane solution was added, and the mixture was stirred at room temperature for 10 hours. After the reaction, the insolubles were filtered off, and the filtrate was concentrated under reduced pressure. The residue was separated by silica gel column chromatography using a mixture of chloroform, methanol and conc. ammonia water (conc. 25% by weight) in the volume ratio 90:9:1 as the eluent. The desired fraction was concentrated under reduced pressure to give 0.38 g (76%) of 4-[4-[(4-chlorophenyl)-2-pyridylmethoxy]-1-piperidyl]butanamide as an oil.

後処理

  1. additionwas added
  2. customAfter the reaction
  3. filtrationthe insolubles were filtered off
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue was separated by silica gel column chromatography
  6. additiona mixture of chloroform, methanol and conc. ammonia water (conc. 25% by weight) in the volume ratio 90:9:1 as the eluent
  7. concentrationThe desired fraction was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-a956e29214ce4fe8a8f381c312d770b1
出典データセット
uspto-grants-1990_05
特許番号
US04929618

関連ノート

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