tert-Butanol → HCID 46253561, 화합물

HRID 1713109

반응식

HRID 1713109 반응식
Br.[N:2]1([C:8]([NH2:10])=[NH:9])[CH2:7][CH2:6][O:5][CH2:4][CH2:3]1.[C:11]([O:15][C:16]([N:18]1[CH2:23][CH2:22][C:21](=O)[C:20](=[CH:25]N(C)C)[CH2:19]1)=[O:17])([CH3:14])([CH3:13])[CH3:12].CC(C)([O-])C.[K+].C(O)(C)(C)C>CCO>[C:11]([O:15][C:16]([N:18]1[CH2:23][CH2:22][C:21]2[N:9]=[C:8]([N:2]3[CH2:7][CH2:6][O:5][CH2:4][CH2:3]3)[N:10]=[CH:25][C:20]=2[CH2:19]1)=[O:17])([CH3:14])([CH3:12])[CH3:13]

참가 물질

6

반응물 4

HCID 6386tert-ButanolHCID 2806564Morpholine-4-carboximidamide HydrobromideHCID 23665647Potassium tert-butoxideHCID 53395404tert-butyl 3-[(dimethylamino)methylene]-4-oxotetrahydro-1(2H)-pyridinecarboxylate

생성물 1

HCID 46253561HCID 46253561, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
75 °C

실험 절차

To a 500 ml round bottom flask charged with anhydrous EtOH (150 ml) under nitrogen at 0° C. are added morpholine-4-carboxamidine hydrobromide (10.50 g, 50 mmol), tert-butyl-3-[(dimethylamino)methylene]-4-oxo-1-piperidinecarboxylate (12.7 g, 50 mmol, 1.0 eq.), and potassium t-butoxide in t-butanol (11.0M, 100 ml, 100 mmol, 2.0 eq.). The resulting mixture is stirred at 75° C. for 16 hr. The solvent is evaporated under reduced pressure, and the residue is taken up in DCM (300 ml), washed with water and brine, dried (Na2SO4) and concentrated. The residue is purified by silica gel chromatography (Hexane/EtOAc 1:1) to give the title compound. MS (+VE) m/z 321.1 (M++1).

후처리

  1. customThe solvent is evaporated under reduced pressure
  2. washwashed with water and brine
  3. dry with materialdried (Na2SO4)
  4. concentrationconcentrated
  5. customThe residue is purified by silica gel chromatography (Hexane/EtOAc 1:1)

출처 및 근거

ORD 기록
ord-7a1b2c88050e4b0d8a190e35d0435036
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07795262B2

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