Triethylamine → 2-Acetyl-7-methoxy-N-[3-pyridylmethyl]-4-benzofuransulphonamide

HRID 965171ノート

反応式

HRID 965171 の反応式
C(N(CC)CC)C.[C:8]([C:11]1[O:12][C:13]2[C:14](=[C:16]([S:22](Cl)(=[O:24])=[O:23])[CH:17]=[CH:18][C:19]=2[O:20][CH3:21])[CH:15]=1)(=[O:10])[CH3:9].[NH2:26][CH2:27][C:28]1[CH:29]=[N:30][CH:31]=[CH:32][CH:33]=1>ClCCl>[C:8]([C:11]1[O:12][C:13]2[C:14](=[C:16]([S:22]([NH:26][CH2:27][C:28]3[CH:29]=[N:30][CH:31]=[CH:32][CH:33]=3)(=[O:24])=[O:23])[CH:17]=[CH:18][C:19]=2[O:20][CH3:21])[CH:15]=1)(=[O:10])[CH3:9]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 310183-PyridinemethanamineHCID 138514332-Acetyl-7-methoxy-4-benzofuransulphonyl chloride

生成物 1

HCID 190759662-Acetyl-7-methoxy-N-[3-pyridylmethyl]-4-benzofuransulphonamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Triethylamine (0.43 ml) was added to a solution of 2-acetyl-7-methoxy-4-benzofuransulphonyl chloride (600 mg) and 3-(aminomethyl)pyridine (0.25 ml) in dichloromethane at room temperature. The resultant mixture was stirred for 20 hours and then diluted with dichloromethane (20 ml). The solution was washed with water (20 ml) and brine (20 ml) and dried (MgSO4). Concentration in vacuo provided a dark oil which was applied to a silica column and eluted with 2% methanol in dichloromethane. The title compound was obtained as a pale yellow solid (161 mg). Mp 168°-170° C.

後処理

  1. washThe solution was washed with water (20 ml) and brine (20 ml)
  2. dry with materialdried (MgSO4)
  3. concentrationConcentration in vacuo
  4. customprovided a dark oil which
  5. washeluted with 2% methanol in dichloromethane

出典と根拠

ORDレコード
ord-f9116923a9c04a33ba82d4bf0aa16ade
出典データセット
uspto-grants-1998_06
特許番号
US05773467

反応ノート

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