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1,4-Dioxane hydrochloride → HCID 178462018、化合物

HRID 1691695
ノート
印刷プレビュー

反応式

HRID 1691695 の反応式
[F:1][C:2]1[CH:7]=[C:6]([C:8]2[NH:12][N:11]=[N:10][N:9]=2)[CH:5]=[C:4]([F:13])[C:3]=1[N:14]1[CH2:19][CH2:18][CH:17]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:16]([CH2:26][N:27]([C@@H:35]([C:37]2[C:46]3[C:41](=[CH:42][CH:43]=[CH:44][CH:45]=3)[CH:40]=[CH:39][CH:38]=2)[CH3:36])C(=O)OC(C)(C)C)[CH2:15]1.[ClH:47].O1CCOCC1>O1CCOCC1>[ClH:47].[F:1][C:2]1[CH:7]=[C:6]([C:8]2[NH:12][N:11]=[N:10][N:9]=2)[CH:5]=[C:4]([F:13])[C:3]=1[N:14]1[CH2:19][CH2:18][CH:17]([C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH:16]([CH2:26][NH:27][C@@H:35]([C:37]2[C:46]3[C:41](=[CH:42][CH:43]=[CH:44][CH:45]=3)[CH:40]=[CH:39][CH:38]=2)[CH3:36])[CH2:15]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 204431481,4-Dioxane hydrochlorideHCID 178461651HCID 178461651、化合物

生成物 1

HCID 178462018HCID 178462018、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To 206 mg of the crude product of tert-butyl ({1-[2,6-difluoro-4-(1H-tetrazol-5-yl)phenyl]-4-phenylpiperidin-3-yl}methyl)[(1R)-1-(1-naphthyl)ethyl]carbamate were added 2.0 mL of 1,4-dioxane and 2.0 mL of a 4 M hydrogen chloride/1,4-dioxane solution, followed by stirring at room temperature for 2 days. The reaction mixture was concentrated under reduced pressure, and to the residue were then added ethyl acetate and a small amount of ethanol, followed by heating for dissolution. Hexane was added thereto, and the precipitate was isolated by filtration, and dried under reduced pressure to obtain 153 mg of (1R)—N-({1-[2,6-difluoro-4-(1H-tetrazol-5-yl)phenyl]-4-phenylpiperidin-3-yl}methyl)-1-(1-naphthyl)ethaneamine hydrochloride as a beige solid.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. temperatureby heating for dissolution
  3. additionHexane was added
  4. customthe precipitate was isolated by filtration
  5. customdried under reduced pressure

出典と根拠

ORDレコード
ord-5a7991b040434d7d9440e36f5497f5c8
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08153658B2

反応ノート

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