Ethanol → (2R,4S,4aS)-11-fluoro-2,4-dimethyl-8-(2-(methylthio)pyrimidin-4-yl)-2,4,4a,6-tetrahydro-1H,1'H-spiro[isoxazolo[4,5-g][1,4]oxazino[4,3-a]quinoline-5,5'-pyrimidine]-2',4',6'(3'H)-trione

HRID 578026

反応式

HRID 578026 の反応式
[CH3:1][C@@H:2]1[CH2:7][N:6]([C:8]2[C:24]([CH:25]=O)=[CH:23][C:11]3[C:12]([C:15]4[CH:20]=[CH:19][N:18]=[C:17]([S:21][CH3:22])[N:16]=4)=[N:13][O:14][C:10]=3[C:9]=2[F:27])[CH2:5][C@@H:4]([CH3:28])[O:3]1.[NH:29]1[C:34](=[O:35])[NH:33][C:32](=[O:36])N[C:30]1=[O:37].[CH3:38]CO>>[F:27][C:9]1[C:10]2[O:14][N:13]=[C:12]([C:15]3[CH:20]=[CH:19][N:18]=[C:17]([S:21][CH3:22])[N:16]=3)[C:11]=2[CH:23]=[C:24]2[C:8]=1[N:6]1[CH2:7][C@@H:2]([CH3:1])[O:3][C@@H:4]([CH3:28])[C@@H:5]1[C:38]1([C:32](=[O:36])[NH:33][C:34](=[O:35])[NH:29][C:30]1=[O:37])[CH2:25]2

参加物

4

反応物 3

HCID 702EthanolHCID 7956Cyanuric acidHCID 867178676-((2R,6R)-2,6-dimethylmorpholino)-7-fluoro-3-(2-(methylthio)pyrimidin-4-yl)benzo[d]isoxazole-5-carbaldehyde2 回

生成物 1

HCID 67434098(2R,4S,4aS)-11-fluoro-2,4-dimethyl-8-(2-(methylthio)pyrimidin-4-yl)-2,4,4a,6-tetrahydro-1H,1'H-spiro[isoxazolo[4,5-g][1,4]oxazino[4,3-a]quinoline-5,5'-pyrimidine]-2',4',6'(3'H)-trione

実験手順

In a microwave reactor, 6-((2R,6R)-2,6-dimethylmorpholino)-7-fluoro-3-(2-(methylthio)pyrimidin-4-yl)benzo[d]isoxazole-5-carbaldehyde (Intermediate 437, 719 mg, 1.79 mmol) and 1,3,5-triazinane-2,4,6-trione (242 mg, 1.88 mmol) in EtOH (10 ml) were heated at 140° C. for 1 hour. The solution was concentrated to dryness to afford 916 mg of desired product, used in subsequent reactions without further purification.

後処理

  1. concentrationThe solution was concentrated to dryness

出典と根拠

ORDレコード
ord-cdf1de1cf71d4a918e0f9455157cf650
出典データセット
uspto-grants-2015_05
特許番号
US09040528B2

関連ノート

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