Water → HCID 23364255、化合物

HRID 1081496ノート

反応式

HRID 1081496 の反応式
[H-].[Na+].[CH2:3]([O:5][C:6]1[CH:23]=[CH:22][C:9]2[NH:10][C:11](=[O:21])[N:12]([C:13]([CH3:20])([CH3:19])[CH2:14][C:15]([CH3:18])([CH3:17])[CH3:16])[C:8]=2[CH:7]=1)[CH3:4].[CH3:24][O:25][C:26]1[CH:31]=[C:30]([N+:32]([O-:34])=[O:33])[CH:29]=[CH:28][C:27]=1[S:35](Cl)(=[O:37])=[O:36].O>C1COCC1.CN(C=O)C>[CH2:3]([O:5][C:6]1[CH:23]=[CH:22][C:9]2[N:10]([S:35]([C:27]3[CH:28]=[CH:29][C:30]([N+:32]([O-:34])=[O:33])=[CH:31][C:26]=3[O:25][CH3:24])(=[O:36])=[O:37])[C:11](=[O:21])[N:12]([C:13]([CH3:20])([CH3:19])[CH2:14][C:15]([CH3:17])([CH3:16])[CH3:18])[C:8]=2[CH:7]=1)[CH3:4]

参加物

7

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 3094582-Methoxy-4-nitrobenzenesulfonyl chlorideHCID 22922482HCID 22922482、化合物

生成物 1

HCID 23364255HCID 23364255、化合物収率 63.2%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

0.2 g of sodium hydride as a 60% dispersion in oil is added in portions to a solution of 1 g of 5-ethoxy-1,3-dihydro-3-(1,1,3,3-tetramethylbutyl)-2H- benzimidazol-2-one in 10 ml of THF and 20 ml of DMF and the mixture is stirred for 30 minutes at RT. 1.2 g of 2-methoxy-4-nitrobenzenesulfonyl chloride are then added and the mixture is stirred for 5 hours at RT. The reaction mixture is poured into 200 ml of water, extracted with AcOEt, washed with water and dried over Na2SO4 and the solvent is evaporated off under vacuum to give 1.1 g of the expected product after crystallization from iso ether. M.p.=158° C.

後処理

  1. stirringthe mixture is stirred for 5 hours at RT
  2. extractionextracted with AcOEt
  3. washwashed with water
  4. dry with materialdried over Na2SO4
  5. customthe solvent is evaporated off under vacuum

出典と根拠

ORDレコード
ord-da824efafad944beb41a84cc2c041117
出典データセット
uspto-grants-1996_12
特許番号
US05585394

反応ノート

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