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

HRID 460385노트

반응식

HRID 460385 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]C)[C:38]([O:44][CH2:45]C)=[C:37]([O:47][CH2:48]C)[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]C)[C:9]=1[O:10][CH2:11]C)[CH2:2]C.[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].[CH3:42][O:41][C:39]1[CH:40]=[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:5]=[C:4]([O:1][CH3:2])[C:9]([O:10][CH3:11])=[C:8]([O:13][CH3:14])[CH:7]=5)=[CH:21][N:20]=4)[CH2:23][CH2:24]3)=[N:30][CH:31]=2)[CH:36]=[C:37]([O:47][CH3:48])[C:38]=1[O:44][CH3:45]

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 206349231,4-Bis[5-(3,4,5-trimethoxyphenyl)-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-534abca251724eb981061ce671bae7b1
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07196101B2

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