Hydrochloric Acid → {3-Amino-5-[4-(trifluoromethyl)phenyl]piperidin-1-yl}(1,4-dioxa-8-azaspiro[4.5]dec-8-yl)methanone hydrochloride

HRID 876257ノート

反応式

HRID 876257 の反応式
[ClH:1].[O:2]1[C:6]2([CH2:11][CH2:10][N:9]([C:12]([N:14]3[CH2:19][CH:18]([C:20]4[CH:25]=[CH:24][C:23]([C:26]([F:29])([F:28])[F:27])=[CH:22][CH:21]=4)[CH2:17][CH:16]([NH:30]C(=O)OC(C)(C)C)[CH2:15]3)=[O:13])[CH2:8][CH2:7]2)[O:5][CH2:4][CH2:3]1>O1CCOCC1>[ClH:1].[NH2:30][CH:16]1[CH2:17][CH:18]([C:20]2[CH:25]=[CH:24][C:23]([C:26]([F:28])([F:29])[F:27])=[CH:22][CH:21]=2)[CH2:19][N:14]([C:12]([N:9]2[CH2:8][CH2:7][C:6]3([O:2][CH2:3][CH2:4][O:5]3)[CH2:11][CH2:10]2)=[O:13])[CH2:15]1

参加物

4

反応物 2

HCID 313Hydrochloric Acid2 回HCID 68075238tert-Butyl {1-(1,4-dioxa-8-azaspiro[4.5]dec-8-ylcarbonyl)-5-[4-(trifluoromethyl)phenyl]piperidin-3-yl}carbamate

生成物 1

HCID 66760651{3-Amino-5-[4-(trifluoromethyl)phenyl]piperidin-1-yl}(1,4-dioxa-8-azaspiro[4.5]dec-8-yl)methanone hydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

37 ml of a 4 N solution of hydrochloric acid in dioxane were added to the carbamate from Example 61A (5.30 g, 7.33 mmol), and the mixture was then stirred at RT for 1 h. Another 37 ml of a 4 N hydrochloric acid solution in dioxane were added, and the mixture was stirred at 60° C. for 3 h. The reaction solution was concentrated under reduced pressure and the residue was taken up in 1 N aqueous hydrogen chloride solution. After washing of the aqueous phase with diethyl ether, the aqueous phase was concentrated under reduced pressure. The crude product obtained in this manner was used further without further purification. Yield: 3.20 g (92% of theory)

後処理

  1. stirringthe mixture was stirred at 60° C. for 3 h
  2. concentrationThe reaction solution was concentrated under reduced pressure
  3. washAfter washing of the aqueous phase with diethyl ether
  4. concentrationthe aqueous phase was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-32da3dc1156d46ba9e0b2b0585ff89d5
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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