Ethylmorpholine → HCID 86761448、化合物

HRID 655202ノート

反応式

HRID 655202 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 86761448HCID 86761448、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e1a2af46a098420786f22507da9aabc3
出典データセット
uspto-grants-2011_12
特許番号
US08071587B2

反応ノート

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