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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Morpholine → 1-((3R,4R)-3-hydroxy-4-(6-methyl-4-morpholin-4-ylpyridin-2-ylamino)pyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone

HRID 1666613
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HRID 1666613 반응식
NN1CCCC1.Cl[C:8]1[CH:13]=[C:12]([CH3:14])[N:11]=[C:10]([NH:15][C@H:16]2[C@H:20]([OH:21])[CH2:19][N:18]([C:22](=[O:35])[CH2:23][C:24]3[CH:29]=[CH:28][C:27]([O:30][C:31]([F:34])([F:33])[F:32])=[CH:26][CH:25]=3)[CH2:17]2)[CH:9]=1.[NH:36]1[CH2:41][CH2:40][O:39][CH2:38][CH2:37]1.CC(C)([O-])C.[Na+].C(P(C(C)(C)C)C1C=CC=CC=1C1C=CC=CC=1)(C)(C)C>C(Cl)(Cl)Cl.CC([O-])=O.CC([O-])=O.[Pd+2].C1(C)C=CC=CC=1>[OH:21][C@H:20]1[C@H:16]([NH:15][C:10]2[CH:9]=[C:8]([N:36]3[CH2:41][CH2:40][O:39][CH2:38][CH2:37]3)[CH:13]=[C:12]([CH3:14])[N:11]=2)[CH2:17][N:18]([C:22](=[O:35])[CH2:23][C:24]2[CH:29]=[CH:28][C:27]([O:30][C:31]([F:34])([F:33])[F:32])=[CH:26][CH:25]=2)[CH2:19]1
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참가 물질

9

반응물 5

HCID 8083MorpholineHCID 279461-PyrrolidinamineHCID 27342152-(Di-tert-butylphosphino)biphenylHCID 23676156Sodium t-butoxideHCID 579701641-((3R,4R)-3-(4-chloro-6-methylpyridin-2-ylamino)-4-hydroxypyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone

생성물 1

HCID 57970145
1-((3R,4R)-3-hydroxy-4-(6-methyl-4-morpholin-4-ylpyridin-2-ylamino)pyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone

시약·촉매·용매 3

HCID 167845palladium(II) acetate촉매HCID 1140Toluene용매HCID 6212Chloroform용매

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온도
100 °C

실험 절차

A mixture of 2,4-dichloro-6-methylpyridine 1-oxide (200 mg), 1-((3R,4R)-3-amino-4-hydroxypyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone (340 mg), and n-butanol (0.6 mL) was stirred at 130° C. for 10 h. The reaction mixture was concentrated under reduced pressure, the residue was purified by silica gel column chromatography (NH silica gel, ethyl acetate−ethyl acetate/methanol=20:1), and then the resulting solids were washed with hexane and diethyl ether to obtain 1-((3R,4R)-3-(4-chloro-6-methylpyridin-2-ylamino)-4-hydroxypyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone (75 mg). (2) A mixture of 1-((3R,4R)-3-(4-chloro-6-methylpyridin-2-ylamino)-4-hydroxypyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone (68 mg), morpholine (0.02 mL), sodium t-butoxide (42 mg), Pd(OAc)2 (1 mg), 2-(di-t-butylphosphino)biphenyl (3 mg), and toluene (1 mL) was heated at 100° C. for 10 h. The mixture was cooled to room temperature, then the reaction mixture was diluted with chloroform, insoluble matters were removed by Celite filtration, and then the filtrate was concentrated under reduced pressure. The residue was purified by preparative TLC (NH silica gel, ethyl acetate, and silica gel, hexane/acetone=1:1) to obtain the title compound (8 mg).

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. customwere removed by Celite filtration
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe residue was purified by preparative TLC (NH silica gel, ethyl acetate, and silica gel, hexane/acetone=1:1)

출처 및 근거

ORD 기록
ord-9f4d7ea3dfaf4720b4d8222912b1343d
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08044068B2

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