Water → HCID 86752188、化合物

HRID 1488

反応式

HRID 1488 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([N:9]=[C:10]2[N:14]3[CH2:15][CH2:16][CH2:17][CH2:18][N:13]3[C:12](=[O:19])[S:11]2)=[CH:4][C:3]=1[N:20]1[C:25](=[O:26])[NH:24][C:23](=[O:27])[N:22]([CH2:28][C:29]([O:31][CH:32]([CH3:34])[CH3:33])=[O:30])[C:21]1=[O:35].C(=O)([O-])[O-].[K+].[K+].Br[CH2:43][C:44]([O:46][CH:47]([CH3:49])[CH3:48])=[O:45].O>CN(C)C=O>[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([N:9]=[C:10]2[N:14]3[CH2:15][CH2:16][CH2:17][CH2:18][N:13]3[C:12](=[O:19])[S:11]2)=[CH:4][C:3]=1[N:20]1[C:25](=[O:26])[N:24]([CH2:43][C:44]([O:46][CH:47]([CH3:49])[CH3:48])=[O:45])[C:23](=[O:27])[N:22]([CH2:28][C:29]([O:31][CH:32]([CH3:33])[CH3:34])=[O:30])[C:21]1=[O:35]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 121593Isopropyl bromoacetateHCID 19690745isopropyl 3-{2-chloro-4-fluoro-5-[(tetrahydro-3-oxo-1H,3H-[1,3,4]thiadiazolo[3,4-a]-pyridazin-1-ylidene)amino]phenyl}tetrahydro-2,4,6-trioxo-s-triazine-1(2H)-acetate

生成物 1

HCID 86752188HCID 86752188、化合物収率 29.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of isopropyl 3-{2-chloro-4-fluoro-5-[(tetrahydro-3-oxo-1H,3H-[1,3,4]thiadiazolo[3,4-a]-pyridazin-1-ylidene)amino]phenyl}tetrahydro-2,4,6-trioxo-s-triazine-1(2H)-acetate (0.85 g, 1.62 mmol), potassium carbonate (0.27 g, 1.95 mmol) and isopropyl bromoacetate (0,353 g, 1.95 mmol)in N,N-dimethylformamide is stirred overnight at room temperature and poured into water. The aqueous mixture is extracted with ethyl acetate. The organic extract is washed with brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to obtain an orange gel. Flash column chromatography of the gel using silica gel and an ethyl acetate/hexanes solution (2:3) gives the title product as a yellow gel (0.3 g) which is identified by NMR spectral analysis.

後処理

  1. extractionThe aqueous mixture is extracted with ethyl acetate
  2. extractionThe organic extract
  3. washis washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customto obtain an orange gel

出典と根拠

ORDレコード
ord-7a8f9c1c64f84e7eae13346d27dfc137
出典データセット
uspto-grants-1998_03
特許番号
US05726126

関連ノート

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