Isopropyl Acetate → (6-Chloro-pyridin-3-yl)-(4-cyclobutyl-[1,4]diazepan-1-yl)-methanone

HRID 404547노트

반응식

HRID 404547 반응식
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([C:8]([N:10]2[CH2:16][CH2:15][CH2:14][N:13]([CH:17]3[CH2:20][CH2:19][CH2:18]3)[CH2:12][CH2:11]2)=[O:9])=[CH:4][CH:3]=1.C(O)(=O)[C@@H]([C@H](C(O)=O)O)O.C(OC(C)=O)(C)C.[OH-].[Na+]>>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([C:8]([N:10]2[CH2:16][CH2:15][CH2:14][N:13]([CH:17]3[CH2:20][CH2:19][CH2:18]3)[CH2:12][CH2:11]2)=[O:9])=[CH:4][CH:3]=1

참가 물질

4

반응물 3

HCID 7915Isopropyl AcetateHCID 14798Sodium HydroxideHCID 86661641(6-chloro-pyridin-3-yl)-(4-cyclobutyl-[1,4]diazepan-1-yl)-methanone L-tartaric acid

생성물 1

HCID 58076653(6-Chloro-pyridin-3-yl)-(4-cyclobutyl-[1,4]diazepan-1-yl)-methanone

실험 절차

A mixture of (6-chloro-pyridin-3-yl)-(4-cyclobutyl-[1,4]diazepan-1-yl)-methanone-L-tartaric acid (172 g, 386.9 mmol), iPrOAc (1.5 L), and 1 N NaOH(aq) (1.5 L) was thoroughly mixed and the resulting layers were separated. The aqueous layer was extracted with additional iPrOAc (1.5 L) and the combined organic layers were dried over magnesium sulfate. After filtration and concentration, (6-chloro-pyridin-3-yl)-(4-cyclobutyl-[1,4]diazepam-1-yl)-methanone was obtained as a yellow oil.

후처리

  1. additionwas thoroughly mixed
  2. customthe resulting layers were separated
  3. extractionThe aqueous layer was extracted with additional iPrOAc (1.5 L)
  4. dry with materialthe combined organic layers were dried over magnesium sulfate
  5. filtrationAfter filtration and concentration
  6. custom(6-chloro-pyridin-3-yl)-(4-cyclobutyl-[1,4]diazepam-1-yl)-methanone was obtained as a yellow oil

출처 및 근거

ORD 기록
ord-f2618380e71d4719ae59d15897339bce
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08748596B2

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