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Sodium hydride → HCID 15388570、化合物

HRID 612396
ノート
印刷プレビュー

反応式

HRID 612396 の反応式
[S:1]1[CH:5]=[CH:4][N:3]=[C:2]1[N:6]1[C:10](=[O:11])[C:9]2([CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]2)[NH:8][C:7]1=[O:17].[H-].[Na+].I[CH2:21][CH2:22][CH3:23]>CN(C)C=O.O>[CH2:21]([N:8]1[C:9]2([CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]2)[C:10](=[O:11])[N:6]([C:2]2[S:1][CH:5]=[CH:4][N:3]=2)[C:7]1=[O:17])[CH2:22][CH3:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 24758Sodium hydrideHCID 336431-IodopropaneHCID 102206081,3-Diazaspiro(4.5)decane-2,4-dione, 3-(2-thiazolyl)-

生成物 1

HCID 15388570HCID 15388570、化合物収率 67%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

5.05 g of the product from Example 2, stage 2 were dissolved in 20 ml of dimethylformamide. 1.10 g of sodium hydride (50% suspension in mineral oil) were added in portions with stirring at 200C. After 1 hour's stirring, 4 ml of 1-iodopropane were added. Stirring was continued for a further 3 hours. The mixture was then diluted with 100 ml of distilled water, extracted three times with 30 ml portions of ethyl acetate, washed with saturated sodium chloride solution and dried over sodium sulphate. Once the solvent had been removed by distillation, the residue was purified by passage through a silica gel column with ethyl acetate/n-hexane=8/5. 3.95 g of l-propyl-3-thiazol-2-yl-1,3-diazaspiro[4.5]decane-2,4-dione (67% of th.) were obtained in the form of white crystals (mp 135-138° C.).

後処理

  1. stirringStirring
  2. waitwas continued for a further 3 hours
  3. extractionextracted three times with 30 ml portions of ethyl acetate
  4. washwashed with saturated sodium chloride solution
  5. dry with materialdried over sodium sulphate
  6. customOnce the solvent had been removed by distillation
  7. customthe residue was purified by passage through a silica gel column with ethyl acetate/n-hexane=8/5

出典と根拠

ORDレコード
ord-34f50492f9254917b0ec8d7921352f4c
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06004963

反応ノート

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