Ethylmorpholine → HCID 86761448, 화합물

HRID 655202노트

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HRID 655202 반응식
[CH:1]([N:3](C1C=CC(F)=CC=1)[CH2:4][C:5]([OH:7])=O)=[O:2].CO[C:17]1[C:25]([O:26][CH3:27])=[CH:24][CH:23]=[CH:22][C:18]=1[CH2:19][CH2:20][NH2:21].C(N1C[CH2:34][O:33]CC1)C.CN(C(ON1N=N[C:46]2[CH:47]=[CH:48][CH:49]=[CH:50][C:45]1=2)=[N+](C)C)C.[B-](F)(F)(F)[F:54]>CN(C=O)C>[CH3:27][O:26][C:25]1[CH:17]=[C:18]([CH2:19][CH2:20][NH:21][C:5](=[O:7])[CH:4]([C:45]2[CH:46]=[CH:47][C:48]([F:54])=[CH:49][CH:50]=2)[NH:3][CH:1]=[O:2])[CH:22]=[CH:23][C:24]=1[O:33][CH3:34]

참가 물질

6

반응물 4

HCID 7525EthylmorpholineHCID 1378582,3-DimethoxyphenethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 86761449HCID 86761449, 화합물

생성물 1

HCID 86761448HCID 86761448, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a mixture of N-formyl-4-fluorophenylglycine (900 mg) and 2,3-dimethoxyphenethylamine (1 ml) in DMF (5 ml) was added N-ethylmorpholine (0.75 ml) and TBTU (1.6 g). After stirring for 4 h, the reaction was quenched by addition of water (30 ml). The product was extracted with ethylacetate. The organic layer was washed with water, dried (MgSO4), filtered and concentrated in vacuo. The residue was triturated with methyl-tert.butylether and recrystallized from toluene.

후처리

  1. customthe reaction was quenched by addition of water (30 ml)
  2. extractionThe product was extracted with ethylacetate
  3. washThe organic layer was washed with water
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue was triturated with methyl-tert.butylether
  8. customrecrystallized from toluene

출처 및 근거

ORD 기록
ord-e1a2af46a098420786f22507da9aabc3
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08071587B2

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