Sulfuric 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 sulfate

HRID 421372노트

반응식

HRID 421372 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].[S:38](=[O:42])(=[O:41])([OH:40])[OH:39]>C(O)C>[S:38]([OH:42])([OH:41])(=[O:40])=[O:39].[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 1118Sulfuric 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 547561695-{8-[(3S)-4-acetyl-3-methylpiperazin-1-yl]-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-2-yl}pyrimidin-2-amine sulfate수율 87.8%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
50 °C

실험 절차

To a suspension 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 (48.7 mg, 0.09 mmol) in 10% aqueous ethanol solution (1 ml) was added 98% sulfuric acid (5.44 μL, 0.09 mmol) at room temperature, and the mixture was heated up to 50° C., then allowed to be cooled down to r.t., and stirred for 5 hr. The solid precipitated out was collected and 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 sulfate (48.9 mg) as a yellow solid.

후처리

  1. temperatureto be cooled down to r.t.
  2. customThe solid precipitated out
  3. customwas collected
  4. customdried

출처 및 근거

ORD 기록
ord-a7513cfd8fa645b59e074dae3e421c9d
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08097622B2

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