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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Triethylamine → (8S)-9-(3-methyl-2-oxobutyl)-2-(1S,4S)-2-oxa-5-azabicyclo[2.2.1]hept-5-yl-8-trifluoromethyl-6,7,8,9-tetrahydropyrimido[1,2-a]pyrimidin-4-one

HRID 633704
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HRID 633704 반응식
Cl[C:2]1[N:3]=[C:4]2[N:12]([CH2:13][C:14](=[O:18])[CH:15]([CH3:17])[CH3:16])[C@H:11]([C:19]([F:22])([F:21])[F:20])[CH2:10][CH2:9][N:5]2[C:6](=[O:8])[CH:7]=1.Cl.[C@H:24]12[CH2:30][C@H:27]([NH:28][CH2:29]1)[CH2:26][O:25]2.C(N(CC)CC)C>C(OCC)(=O)C>[CH3:16][CH:15]([CH3:17])[C:14](=[O:18])[CH2:13][N:12]1[C:4]2=[N:3][C:2]([N:28]3[CH2:29][C@@H:24]4[CH2:30][C@H:27]3[CH2:26][O:25]4)=[CH:7][C:6](=[O:8])[N:5]2[CH2:9][CH2:10][C@H:11]1[C:19]([F:22])([F:21])[F:20]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 21303398(1S,4S)-2-oxa-5-azabicyclo(2.2.1)heptane hydrochlorideHCID 118194457(8S)-2-chloro-9-(3-methyl-2-oxobutyl)-8-trifluoromethyl-6,7,8,9-tetrahydropyrimido[1,2-a]pyrimidin-4-one

생성물 1

HCID 72708977(8S)-9-(3-methyl-2-oxobutyl)-2-(1S,4S)-2-oxa-5-azabicyclo[2.2.1]hept-5-yl-8-trifluoromethyl-6,7,8,9-tetrahydropyrimido[1,2-a]pyrimidin-4-one수율 49%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
130 °C

실험 절차

220 mg (0.51 mmol) of (8S)-2-chloro-9-(3-methyl-2-oxobutyl)-8-trifluoromethyl-6,7,8,9-tetrahydropyrimido[1,2-a]pyrimidin-4-one and 105.99 mg (0.78 mmol) of (1S,4S)-2-oxa-5-azabicyclo[2.2.1]heptane hydrochloride are mixed together. The powder obtained is placed in a tube and 227 μl (1.63 mmol) of triethylamine are added. The tube is sealed and heated at 130° C. in an oil bath for 3 hours. The crude product obtained is taken up in ethyl acetate and the organic phase is washed with water, dried over magnesium sulfate and then evaporated to dryness. The residue is purified by chromatography on silica gel (eluent: 95/5 EtOAc/MeOH) to give 100 mg of (8S)-9-(3-methyl-2-oxobutyl)-2-(1S,4S)-2-oxa-5-azabicyclo[2.2.1]hept-5-yl-8-trifluoromethyl-6,7,8,9-tetrahydropyrimido[1,2-a]pyrimidin-4-one, the characteristics of which are as follows:

후처리

  1. customThe powder obtained
  2. customis placed in a tube
  3. customThe tube is sealed
  4. customThe crude product obtained
  5. washthe organic phase is washed with water
  6. dry with materialdried over magnesium sulfate
  7. customevaporated to dryness
  8. customThe residue is purified by chromatography on silica gel (eluent: 95/5 EtOAc/MeOH)

출처 및 근거

ORD 기록
ord-d199ad387da34cb993a55dfac3b46318
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09321790B2

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