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1,4-Dioxane hydrochloride → HCID 68758453, 화합물

HRID 2382204
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HRID 2382204 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 204431481,4-Dioxane hydrochlorideHCID 68733962HCID 68733962, 화합물

생성물 1

HCID 68758453HCID 68758453, 화합물수율 84.1%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3af992a60d244c5996f1545e93914578
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08258306B2

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