Water → HCID 23364255, 화합물

HRID 1081496노트

반응식

HRID 1081496 반응식
[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]

참가 물질

7

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 3094582-Methoxy-4-nitrobenzenesulfonyl chlorideHCID 22922482HCID 22922482, 화합물

생성물 1

HCID 23364255HCID 23364255, 화합물수율 63.2%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-da824efafad944beb41a84cc2c041117
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05585394

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