Sodium hydride → HCID 131726208、化合物

HRID 1374790ノート

反応式

HRID 1374790 の反応式
[H-].[Na+].[Cl:3][C:4]1[CH:9]=[CH:8][C:7]([S:10][C:11]2[C:19]3[C:18]([C:20]#[N:21])=[C:17]([CH3:22])[CH:16]=[CH:15][C:14]=3[NH:13][C:12]=2[CH3:23])=[CH:6][CH:5]=1.Br[CH2:25][C:26]([O:28][CH3:29])=[O:27]>O1CCCC1>[Cl:3][C:4]1[CH:5]=[CH:6][C:7]([S:10][C:11]2[C:19]3[C:14](=[CH:15][CH:16]=[C:17]([CH3:22])[C:18]=3[C:20]#[N:21])[N:13]([CH2:25][C:26]([O:28][CH3:29])=[O:27])[C:12]=2[CH3:23])=[CH:8][CH:9]=1

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 60984Methyl bromoacetateHCID 210778313-[(4-Chlorophenyl)sulfanyl]-2,5-dimethyl-1H-indole-4-carbonitrile

生成物 1

HCID 131726208HCID 131726208、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a stirred solution of sodium hydride (96.1 mg of 60% dispersion in mineral oil) in dry tetrahydrofuran (15 ml) was added 3-[(4-chlorophenyl)thio]-2,5-dimethyl-1H-indole-4-carbonitrile (400 mg) in dry tetrahydrofuran (5 ml). After 30 minutes the reaction was treated with methyl bromoacetate (177 μl) and stirring continued for 4 hours. The solvent was removed in vacuo, the residue redissolved in ethyl acetate, washed with water, brine, dried (MgSO4), evaporated in vacuo and the residue purified by flash column chromatography eluting with 1:1 ethyl acetate and iso-hexane mixture. The sub-title compound was obtained as a yellow solid (360 mg).

後処理

  1. customThe solvent was removed in vacuo
  2. dissolutionthe residue redissolved in ethyl acetate
  3. washwashed with water, brine
  4. dry with materialdried (MgSO4)
  5. customevaporated in vacuo
  6. customthe residue purified by flash column chromatography
  7. washeluting with 1:1 ethyl acetate and iso-hexane mixture

出典と根拠

ORDレコード
ord-7753c3b46f9b44ed9ae6238e11b9eea5
出典データセット
uspto-grants-2007_01
特許番号
US07166607B2

反応ノート

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