Methanesulfonic Acid → 1,4-Bis[5-(3,4,5-triethoxyphenyl)-2-pyridyl]hexahydro-1,4-diazepine dimethanesulfonate

HRID 49299노트

반응식

HRID 49299 반응식
[O:1]([C:4]1[CH:5]=[C:6]([C:16]2[CH:17]=[CH:18][C:19]([N:22]3[CH2:28][CH2:27][CH2:26][N:25]([C:29]4[CH:34]=[CH:33][C:32]([C:35]5[CH:40]=[C:39]([O:41][CH2:42][CH3:43])[C:38]([O:44][CH2:45][CH3:46])=[C:37]([O:47][CH2:48][CH3:49])[CH:36]=5)=[CH:31][N:30]=4)[CH2:24][CH2:23]3)=[N:20][CH:21]=2)[CH:7]=[C:8]([O:13][CH2:14][CH3:15])[C:9]=1[O:10][CH2:11][CH3:12])[CH2:2][CH3:3].[CH3:50][S:51]([OH:54])(=[O:53])=[O:52]>CO>[CH3:50][S:51]([OH:54])(=[O:53])=[O:52].[CH3:50][S:51]([OH:54])(=[O:53])=[O:52].[CH2:48]([O:47][C:37]1[CH:36]=[C:35]([C:32]2[CH:33]=[CH:34][C:29]([N:25]3[CH2:26][CH2:27][CH2:28][N:22]([C:19]4[CH:18]=[CH:17][C:16]([C:6]5[CH:7]=[C:8]([O:13][CH2:14][CH3:15])[C:9]([O:10][CH2:11][CH3:12])=[C:4]([O:1][CH2:2][CH3:3])[CH:5]=5)=[CH:21][N:20]=4)[CH2:23][CH2:24]3)=[N:30][CH:31]=2)[CH:40]=[C:39]([O:41][CH2:42][CH3:43])[C:38]=1[O:44][CH2:45][CH3:46])[CH3:49]

참가 물질

4

반응물 2

HCID 6395Methanesulfonic AcidHCID 206349381,4-Bis[5-(3,4,5-triethoxylphenyl)-2-pyridyl]hexahydro-1,4-diazepine

생성물 1

HCID 206349391,4-Bis[5-(3,4,5-triethoxyphenyl)-2-pyridyl]hexahydro-1,4-diazepine dimethanesulfonate수율 94%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 1,4-bis[5-(3,4,5-triethoxylphenyl)-2-pyridyl]hexahydro-1,4-diazepine (77 mg, 0.115 mmol) in methanol (5.0 mL) was added a 1.0 M aqueous methanesulfonic acid (0.23 mL, 0.23 mmol), and the reaction mixture was concentrated under reduced pressure. Ethanol (5.0 mL) was added to the residue, and the resulting mixture was concentrated under reduced pressure. The residue was recrystallized from methanol-diethyl ether to yield the title compound as a pale yellow crystalline powder (melting point: 235.0-237.0° C.) (74.0 mg, yield: 94%).

후처리

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. additionEthanol (5.0 mL) was added to the residue
  3. concentrationthe resulting mixture was concentrated under reduced pressure
  4. customThe residue was recrystallized from methanol-diethyl ether

출처 및 근거

ORD 기록
ord-837cc1f0d66546d0a7a435edf2e40bf1
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06706703B2

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