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1,3-Bis(trimethylsilyl)urea → benzhydryl (6R,7R)-7-[[(2Z)-2-acetyloxyimino-2-(2-amino-1,3-thiazol-4-yl)acetyl]amino]-8-oxo-3-(1H-pyrazol-4-ylmethylsulfanyl)-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate

HRID 992707
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인쇄 미리보기

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HRID 992707 반응식
[NH2:1][C@@H:2]1[C:32](=[O:33])[N:4]2[C:5]([C:16]([O:18][CH:19]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)[C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[O:17])=[C:6]([S:9][CH2:10][C:11]3[CH:12]=[N:13][NH:14][CH:15]=3)[CH2:7][S:8][C@H:3]12.C[Si](C)(C)NC(N[Si](C)(C)C)=O.[NH2:46][C:47]1[S:48][CH:49]=[C:50](/[C:52](=[N:56]/[O:57][C:58](=[O:60])[CH3:59])/[C:53](Cl)=[O:54])[N:51]=1.C(=O)(O)[O-].[Na+]>C1COCC1.C(#N)C.C(OCC)(=O)C>[NH2:46][C:47]1[S:48][CH:49]=[C:50](/[C:52](=[N:56]/[O:57][C:58](=[O:60])[CH3:59])/[C:53]([NH:1][C@@H:2]2[C:32](=[O:33])[N:4]3[C:5]([C:16]([O:18][CH:19]([C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=4)[C:26]4[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=4)=[O:17])=[C:6]([S:9][CH2:10][C:11]4[CH:15]=[N:14][NH:13][CH:12]=4)[CH2:7][S:8][C@H:3]23)=[O:54])[N:51]=1
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8

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HCID 875621,3-Bis(trimethylsilyl)ureaHCID 516892Sodium BicarbonateHCID 11322595[(Z)-[1-(2-amino-1,3-thiazol-4-yl)-2-chloro-2-oxoethylidene]amino] acetateHCID 70122266Diphenylmethyl 7beta-amino-3-[(pyrazol-4-yl)methylthio]-3-cephem-4-carboxylate

생성물 1

HCID 88158439
benzhydryl (6R,7R)-7-[[(2Z)-2-acetyloxyimino-2-(2-amino-1,3-thiazol-4-yl)acetyl]amino]-8-oxo-3-(1H-pyrazol-4-ylmethylsulfanyl)-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate

시약·촉매·용매 3

HCID 6342Acetonitrile용매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

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온도
35 °C

실험 절차

Under nitrogen atmosphere, to a suspension of diphenylmethyl 7β-amino-3-[(pyrazol-4-yl)methylthio]-3-cephem-4-carboxylate (30.2 g) in THF (800 ml) was added herein 1,3-bis(trimethylsilyl)urea (25.8 g) was added at the room temperature. The reaction mixture was warmed at 35° C. and dissolved, and then it was cooled below 0° C. A suspension of 2-(2-aminothiazol-4-yl)-2-(Z)-(acetoxyimino)acetylchloride monohydrochiloride salt (17.93 g) in acetonitrile (200 ml) was dropped into the above reaction mixture below 0° C. After stirring at the same temperature for 10 minutes, it was poured into a mixture of ethyl acetate (1.2 l) and ice-water (1.5 l). The aqueous layer was adjusted at pH 6.5 with saturated sodium bicarbonate solution. The organic layer was separated, washed with brine (1.0 l), and dried over magnesium sulfate, and then evaporated until the volume amounted to 500 ml. The solution was poured into IPE (1.5 l). The resulting precipitate was filtered, dried under reduced pressure to give diphenylmethyl 7β-[2-(2-aminothiazol-4-yl)-2-(Z)-(acetoxyimino)acetamido]-3-[(pyrazol-4-yl)methylthio]-3-cephem-4-carboxylate (41.3 g) as powder.

후처리

  1. additionwas added at the room temperature
  2. dissolutiondissolved
  3. temperatureit was cooled below 0° C
  4. additionwas dropped into the above reaction mixture below 0° C
  5. customThe organic layer was separated
  6. washwashed with brine (1.0 l)
  7. dry with materialdried over magnesium sulfate
  8. customevaporated until the volume
  9. additionThe solution was poured into IPE (1.5 l)
  10. filtrationThe resulting precipitate was filtered
  11. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-b7c71077da35489a8f8cb2c4e1afde81
출처 데이터셋
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06468995B1

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