Methanesulfonic Acid → 5-{8-[(3S)-4-acetyl-3-methylpiperazin-1-yl]-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-2-yl}pyrimidin-2-amine methanesulfonate

HRID 421371노트

반응식

HRID 421371 반응식
[C:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[N:11]([CH2:32][C:33]([F:36])([F:35])[F:34])[C:12]3[C:17]([N:18]=2)=[C:16]([N:19]2[CH2:24][CH2:23][O:22][CH2:21][CH2:20]2)[N:15]=[C:14]([C:25]2[CH:26]=[N:27][C:28]([NH2:31])=[N:29][CH:30]=2)[N:13]=3)[CH2:6][C@@H:5]1[CH3:37])(=[O:3])[CH3:2].[CH3:38][S:39]([OH:42])(=[O:41])=[O:40]>CO.ClCCl>[CH3:38][S:39]([OH:42])(=[O:41])=[O:40].[C:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[N:11]([CH2:32][C:33]([F:36])([F:35])[F:34])[C:12]3[C:17]([N:18]=2)=[C:16]([N:19]2[CH2:20][CH2:21][O:22][CH2:23][CH2:24]2)[N:15]=[C:14]([C:25]2[CH:26]=[N:27][C:28]([NH2:31])=[N:29][CH:30]=2)[N:13]=3)[CH2:6][C@@H:5]1[CH3:37])(=[O:3])[CH3:2]

참가 물질

4

반응물 2

HCID 6395Methanesulfonic AcidHCID 453781715-{8-[(3S)-4-acetyl-3-methylpiperazin-1-yl]-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-2-yl}pyrimidin-2-amine

생성물 1

HCID 547560515-{8-[(3S)-4-acetyl-3-methylpiperazin-1-yl]-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-2-yl}pyrimidin-2-amine methanesulfonate수율 84.9%

시약·촉매·용매 1

HCID 21226129Dichloromethane methanol용매

실험 절차

To a solution of 5-{8-[(3S)-4-acetyl-3-methylpiperazin-1-yl]-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-2-yl}pyrimidin-2-amine (33.2 mg, 0.06 mmol) in methanol/dichloromethane solution (1/1, 1 ml) was added methanesulfonic acid (3.9 μl, 0.06 mmol) at room temperature, and the mixture was stirred for 3 hr. Then the solvent was removed in reduced pressure, and the resultant solid was dried to give 5-{8-[(3S)-4-acetyl-3-methylpiperazin-1-yl]-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-2-yl}pyrimidin-2-amine methanesulfonate (31.4 mg) as a yellow solid.

후처리

  1. customThen the solvent was removed in reduced pressure
  2. customthe resultant solid was dried

출처 및 근거

ORD 기록
ord-93a651dee8bb4bc997d04da028b35864
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08097622B2

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