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1,4-Dioxane hydrochloride → HCID 68758453、化合物

HRID 2382204
ノート
印刷プレビュー

反応式

HRID 2382204 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([N:14]3[CH2:19][CH2:18][N:17](C(OC(C)(C)C)=O)[C@H:16]([CH3:27])[CH2:15]3)[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1.Cl.O1CCOCC1>O1CCOCC1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([N:14]3[CH2:19][CH2:18][NH:17][C@H:16]([CH3:27])[CH2:15]3)[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=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 68733962HCID 68733962、化合物

生成物 1

HCID 68758453HCID 68758453、化合物収率 84.1%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a solution of (R)-tert-butyl 4-(1-(4-chlorophenyl)cyclohexyl)-2-methylpiperazine-1-carboxylate (0.80 g, 2.03 mmol) in 1,4-dioxane (5 mL) at 0° C. was added dropwise a saturated solution dioxane-HCl (4 mL). The reaction mixture was warmed to room temperature and stirred for 2 h. The reaction mixture was concentrated under reduced pressure and the residue was washed with ethyl acetate. The pH of the residue was adjusted to 7 using aqueous 10% sodium carbonate solution and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure to afford 0.5 g of (R)-1-(1-(4-chlorophenyl)cyclohexyl)-3-methylpiperazine.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. washthe residue was washed with ethyl acetate
  3. extractionextracted with ethyl acetate
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-3af992a60d244c5996f1545e93914578
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08258306B2

反応ノート

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