Morpholine → HCID 59506284、化合物

HRID 1098763ノート

反応式

HRID 1098763 の反応式
[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]

参加物

8

反応物 4

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

生成物 1

HCID 59506284HCID 59506284、化合物収率 54%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-4c95c90a1d6e4051abd9ed8da27e600a
出典データセット
uspto-grants-2012_03
特許番号
US08143242B2

反応ノート

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