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

HRID 965171노트

반응식

HRID 965171 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f9116923a9c04a33ba82d4bf0aa16ade
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05773467

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