Morpholine → HCID 59506284, 화합물

HRID 1098763노트

반응식

HRID 1098763 반응식
[C:1]([C:4]1[CH:12]=[CH:11][C:7]([C:8]([OH:10])=O)=[C:6]([Br:13])[CH:5]=1)(=[O:3])[CH3:2].[B-](F)(F)(F)F.[CH3:19][CH2:20][O:21][C:22]([C:24](C#N)=[N:25]OC(N(C)C)=[N+](C)C)=O.N1CCOCC1.CCN(C(C)C)C(C)C>CN(C=O)C.O.C(OCC)(=O)C>[Br:13][C:6]1[CH:5]=[C:4]([C:1](=[O:3])[CH3:2])[CH:12]=[CH:11][C:7]=1[C:8]([N:25]1[CH2:19][CH2:20][O:21][CH2:22][CH2:24]1)=[O:10]

참가 물질

8

반응물 4

HCID 8083MorpholineHCID 81531DiisopropylethylamineHCID 2733286O-[(Ethoxycarbonyl)cyanomethylenamino]-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 13347277HCID 13347277, 화합물

생성물 1

HCID 59506284HCID 59506284, 화합물수율 54%

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of the product obtained in step 3 (230 mg, 0.95 mmol) and TOTU (310 mg, 0.95 mmol) in DMF (2 mL) was added morpholine (83 μL, 0.95 mmol) and DIPEA (162 μL, 0.95 mmol). The reaction mixture was stirred for 2 h at RT. Ethyl acetate (20 ml) and water (20 ml) was added, the organic phase was separated and washed with hydrochloric acid (1 M, 20 ml), water (20 ml), brine (2×20 ml) and dried over Na2SO4. After evaporation and flash-chromatography the product was obtained as oil (160 mg, 54%).

후처리

  1. customthe organic phase was separated
  2. washwashed with hydrochloric acid (1 M, 20 ml), water (20 ml), brine (2×20 ml)
  3. dry with materialdried over Na2SO4
  4. customAfter evaporation and flash-chromatography the product

출처 및 근거

ORD 기록
ord-4c95c90a1d6e4051abd9ed8da27e600a
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143242B2

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