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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Hydrochloric Acid → (S)-[1-[[[[3-[[(1,4-Dihydro-5-hydroxy-4-oxo-2-pyridinyl)carbonyl]amino]tetrahydro-2-oxo-1(2H)-pyrimidinyl]sulfonyl]amino]carbonyl]-2-oxo-3-azetidinyl]carbamic acid, phenylmethyl ester

HRID 2351086
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HRID 2351086 반응식
[OH:1][C:2]1[C:3](=[O:18])[CH:4]=[C:5]([C:8]([NH:10][N:11]2[CH2:16][CH2:15][CH2:14][NH:13][C:12]2=[O:17])=[O:9])[NH:6][CH:7]=1.CN([Si](C)(C)C)C(=O)C(F)(F)F.N1CCCNC1=O.[O:38]=[C:39]1[C@@H:42]([NH:43][C:44](=[O:53])[O:45][CH2:46][C:47]2[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=2)[CH2:41][NH:40]1.Cl[S:55]([N:58]=[C:59]=[O:60])(=[O:57])=[O:56].Cl>C(OCC)(=O)C.ClCCl>[OH:1][C:2]1[C:3](=[O:18])[CH:4]=[C:5]([C:8]([NH:10][N:11]2[CH2:16][CH2:15][CH2:14][N:13]([S:55]([NH:58][C:59]([N:40]3[CH2:41][C@H:42]([NH:43][C:44](=[O:53])[O:45][CH2:46][C:47]4[CH:48]=[CH:49][CH:50]=[CH:51][CH:52]=4)[C:39]3=[O:38])=[O:60])(=[O:57])=[O:56])[C:12]2=[O:17])=[O:9])[NH:6][CH:7]=1
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참가 물질

9

반응물 6

HCID 313Hydrochloric AcidHCID 32510N-methyl-N-(trimethylsilyl)trifluoroacetamideHCID 70918Chlorosulfonyl isocyanateHCID 746152(1H)-Pyrimidinone, tetrahydro-2회HCID 12834624benzyl N-[(3S)-2-oxoazetidin-3-yl]carbamateHCID 198480131,4-Dihydro-5-hydroxy-4-oxo-N-(tetrahydro-2-oxo-1(2H)-pyrimidinyl)-2-pyridinecarboxamide

생성물 1

HCID 86743424(S)-[1-[[[[3-[[(1,4-Dihydro-5-hydroxy-4-oxo-2-pyridinyl)carbonyl]amino]tetrahydro-2-oxo-1(2H)-pyrimidinyl]sulfonyl]amino]carbonyl]-2-oxo-3-azetidinyl]carbamic acid, phenylmethyl ester

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매2회

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온도
0 °C

실험 절차

2.73 g (10.82 mmol) 1,4-dihydro-5-hydroxy-4-oxo-N-(tetrahydro-2-oxo-1(2H)-pyrimidinyl)-2-pyridinecarboxamide and 8.63 g (43.29 mmol) N-methyl-N-trimethylsilyltrifluoroacetamide were dissolved in ethyl acetate and stirred for 1 hour (solution A). To a suspension of 2.38 g (10.82 mmol) (S)-(2-oxo-3-azetidinyl)carbamic acid, phenylmethyl ester in 80 ml ethyl acetate was added 1.53 g (10.82 mmol) chlorosulfonyl isocyanate. After stirring for 1 hour, the solution was cooled to 0° C. and 9 ml dichloromethane and subsequently solution A were added. After stirring overnight at room temperature ice water was added and the pH was adjusted to 1.3 with 3N hydrochloric acid. The precipitate was filtered off, washed with water, dried in vacuo and slurried with ether. Yield 4.95 g, melting range 150°-230° C. (dec.).

후처리

  1. additionwas added
  2. filtrationThe precipitate was filtered off
  3. washwashed with water
  4. customdried in vacuo

출처 및 근거

ORD 기록
ord-d6b1ec5eeed344889ebecb40d77e4209
출처 데이터셋
uspto-grants-1989_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04871841

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