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1,4-Dioxane hydrochloride → HCID 117839269, 화합물

HRID 1477636
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HRID 1477636 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:10]2[C@@H:15]([O:16][C:17](=[O:22])[C:18]([CH3:21])([CH3:20])[CH3:19])[CH2:14][N:13](C(OC(C)(C)C)=O)[CH2:12][CH:11]=2)=[N:6][C:7]=1[O:8][CH3:9].Cl.O1CCOCC1>CO>[C:17]([O:16][C@@H:15]1[C:10]([C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[C:7]([O:8][CH3:9])[N:6]=2)=[CH:11][CH2:12][NH:13][CH2:14]1)(=[O:22])[C:18]([CH3:21])([CH3:20])[CH3:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 204431481,4-Dioxane hydrochlorideHCID 117849075HCID 117849075, 화합물

생성물 1

HCID 117839269HCID 117839269, 화합물수율 127.8%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a methanol solution (1.0 mL) of tert-butyl (R)-5-chloro-6-methoxy-5′-(pivaloyloxy)-5′,6′-dihydro-[2,4′-bipyridine]-1′(2′H)-carboxylate (1.35 g, 3.18 mmol) synthesized in Reference Synthesis Example 142, 4 M hydrogen chloride/1,4-dioxane (15 mL) was added and the resultant mixture was stirred at room temperature for 5 minutes. After completion of the reaction, the reaction solution was concentrated under reduced pressure and saturated sodium bicarbonate aqueous solution and water were added to the concentrated solution, followed by extraction from the resultant mixture with ethyl acetate. The organic layer was concentrated under reduced pressure to obtain a crude product of the title compound (1.32 g).

후처리

  1. additionwas added
  2. customAfter completion of the reaction
  3. concentrationthe reaction solution was concentrated under reduced pressure and saturated sodium bicarbonate aqueous solution and water
  4. additionwere added to the concentrated solution
  5. extractionfollowed by extraction from the resultant mixture with ethyl acetate
  6. concentrationThe organic layer was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-cde83dbd09d34a8fad044e25fbbdf49e
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09403798B2

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