tert-Butanol → HCID 178454378、化合物

HRID 1930743ノート

反応式

HRID 1930743 の反応式
[F:1][C:2]1[CH:8]=[C:7]([O:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]3[N:17]=[C:18]([CH2:21][O:22][C:23]4[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=4)[NH:19][CH:20]=3)=[CH:12][CH:11]=2)[CH:6]=[CH:5][C:3]=1[NH2:4].C(N(CC)CC)C.[S:36](Cl)([N:39]=[C:40]=[O:41])(=[O:38])=[O:37].[C:43]([OH:47])([CH3:46])([CH3:45])[CH3:44]>ClCCl>[F:1][C:2]1[CH:8]=[C:7]([O:9][C:10]2[CH:11]=[CH:12][C:13]([C:16]3[N:17]=[C:18]([CH2:21][O:22][C:23]4[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=4)[NH:19][CH:20]=3)=[CH:14][CH:15]=2)[CH:6]=[CH:5][C:3]=1[NH:4][S:36]([NH:39][C:40](=[O:41])[O:47][C:43]([CH3:46])([CH3:45])[CH3:44])(=[O:38])=[O:37]

参加物

6

反応物 4

HCID 6386tert-ButanolHCID 8471TriethylamineHCID 70918Chlorosulfonyl isocyanateHCID 178507749HCID 178507749、化合物

生成物 1

HCID 178454378HCID 178454378、化合物収率 75%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

At 0° C., the compound 2-fluoro-4-{4-[2-(phenoxymethyl)-1H-imidazol-4-yl]phenoxy}aniline (1.5 g, 4 mmol) and triethylamine (0.63 ml, 4.52 mmol) are solubilized in 10 ml of dichloromethane. A mixture containing sulfonyl isocyanate chloride (0.623 g, 4.40 mmol) and tert-butanol (0.325 g, 4.40 mmol) in 10 ml of dichloromethane is added to this solution at 0° C. The reaction medium is returned to ambient temperature then stirred for two hours. After evaporation of the solvent, the solid obtained is purified on a silica column (eluent: dichloromethane-methanol: 95-5). After washing in dichloromethane then filtration, a yellow-coloured powder is obtained with a yield of 75%.

後処理

  1. customAt 0° C.
  2. additionis added to this solution at 0° C
  3. customis returned to ambient temperature
  4. customAfter evaporation of the solvent
  5. customthe solid obtained
  6. customis purified on a silica column (eluent: dichloromethane-methanol: 95-5)
  7. washAfter washing in dichloromethane
  8. filtrationfiltration
  9. customa yellow-coloured powder is obtained with a yield of 75%

出典と根拠

ORDレコード
ord-d838aeeb81784079a5bdbc5a2e383ff0
出典データセット
uspto-grants-2012_05
特許番号
US08188133B2

反応ノート

読み込み中…