Hydrochloric Acid → 1-({3-Amino-5-[4-(trifluoromethyl)phenyl]piperidin-1-yl}carbonyl)piperidine-4-carbonitrile hydrochloride

HRID 876263ノート

反応式

HRID 876263 の反応式
[ClH:1].[C:2]([CH:4]1[CH2:9][CH2:8][N:7]([C:10]([N:12]2[CH2:17][CH:16]([C:18]3[CH:23]=[CH:22][C:21]([C:24]([F:27])([F:26])[F:25])=[CH:20][CH:19]=3)[CH2:15][CH:14]([NH:28]C(=O)OC(C)(C)C)[CH2:13]2)=[O:11])[CH2:6][CH2:5]1)#[N:3]>O1CCOCC1>[ClH:1].[NH2:28][CH:14]1[CH2:15][CH:16]([C:18]2[CH:23]=[CH:22][C:21]([C:24]([F:27])([F:25])[F:26])=[CH:20][CH:19]=2)[CH2:17][N:12]([C:10]([N:7]2[CH2:6][CH2:5][CH:4]([C:2]#[N:3])[CH2:9][CH2:8]2)=[O:11])[CH2:13]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 68075239tert-Butyl {1-[(4-cyanopiperidin-1-yl)carbonyl]-5-[4-(trifluoromethyl)phenyl]piperidin-3-yl}carbamate

生成物 1

HCID 667610061-({3-Amino-5-[4-(trifluoromethyl)phenyl]piperidin-1-yl}carbonyl)piperidine-4-carbonitrile hydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

78 ml of a 4N solution of hydrochloric acid in dioxane were added to 8.30 g (15.7 mmol) of the carbamate from Example 68A having a purity of 91%, and the mixture was stirred at room temperature for 1 h. The reaction solution was concentrated under reduced pressure and the residue was taken up in 1 N hydrochloric acid. After washing with diethyl ether, the organic phase was concentrated under reduced pressure and the residue was taken up in dichloromethane and extracted repeatedly with 1N hydrochloric acid. The combined aqueous phases were concentrated under reduced pressure, and the residue was dried under high vacuum. Yield: 4.93 g (71% of theory)

後処理

  1. concentrationThe reaction solution was concentrated under reduced pressure
  2. washAfter washing with diethyl ether
  3. concentrationthe organic phase was concentrated under reduced pressure
  4. extractionextracted repeatedly with 1N hydrochloric acid
  5. concentrationThe combined aqueous phases were concentrated under reduced pressure
  6. customthe residue was dried under high vacuum

出典と根拠

ORDレコード
ord-86e0e37d0f1649f9a880cdae61ad4f0c
出典データセット
uspto-grants-2015_03
特許番号
US08987248B2

反応ノート

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