Toluene → HCID 178471882、化合物

HRID 477828

反応式

HRID 477828 の反応式
[CH2:1]([O:3][C:4]([N:6]([CH2:8][CH:9]1[CH2:14][N:13]([C:15]2[C:28]([F:29])=[CH:27][C:18]([C:19]([CH2:21][C:22]([O:24][CH2:25][CH3:26])=[O:23])=[O:20])=[C:17]([F:30])[C:16]=2[F:31])[CH2:12][CH2:11][O:10]1)[CH3:7])=[O:5])[CH3:2].CO[CH:34](OC)[N:35]([CH3:37])C.[C:40]1(C)C=CC=C[CH:41]=1>>[CH2:1]([O:3][C:4]([N:6]([CH2:8][CH:9]1[CH2:14][N:13]([C:15]2[C:28]([F:29])=[CH:27][C:18]([C:19]([C:21](=[CH:37][NH:35][CH:34]3[CH2:41][CH2:40]3)[C:22]([O:24][CH2:25][CH3:26])=[O:23])=[O:20])=[C:17]([F:30])[C:16]=2[F:31])[CH2:12][CH2:11][O:10]1)[CH3:7])=[O:5])[CH3:2]

参加物

4

反応物 3

HCID 1140TolueneHCID 78373Dimethylformamide dimethyl acetalHCID 14652581ethyl 4-[2-(N-ethoxycarbonyl-N-methylaminomethyl)morpholino]-2,3,5-trifluorobenzoylacetate

生成物 1

HCID 178471882HCID 178471882、化合物収率 89%

実験手順

4.14 (2H, q, J=7Hz), 7.08-7.52 (1H, m) (2) A solution of 4.46 g of ethyl 4-[2-(N-ethoxycarbonyl-N-methylaminomethyl)morpholino]-2,3,5-trifluorobenzoylacetate, 1.85 g of dimethylformamide dimethylacetal and 20 ml of toluene is refluxed for 6 hours. The reaction mixture is concentrated under reduced pressure and to the obtained residue is added 20 ml of ethanol. After the addition of 0.94 g of cyclopropylamine with ice-cooling, the mixture is stirred at room temperature for 3 hours. The reaction mixture is concentrated under reduced pressure and the obtained residue is purified by chromatography on silica gel to give 4.06 g of ethyl 2-[4-[2-(N-ethoxycarbonyl-N-methylaminomethyl)morpholino]-2,3,5-trifluorobenzoyl]-3-cyclopropylaminoacrylate in 89% yield, as an oily substance.

後処理

  1. concentrationThe reaction mixture is concentrated under reduced pressure and to the obtained residue
  2. additionis added 20 ml of ethanol
  3. additionAfter the addition of 0.94 g of cyclopropylamine with ice-
  4. temperaturecooling
  5. concentrationThe reaction mixture is concentrated under reduced pressure
  6. customthe obtained residue is purified by chromatography on silica gel

出典と根拠

ORDレコード
ord-5d2adfb983854fdca9afe5315a07e008
出典データセット
uspto-grants-1989_12
特許番号
US04889857

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