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Cyclohexane → (S)-N-(Methylsulfonyl)-2-oxo-3-[[(phenylmethoxy)-carbonyl]amino]-1-azetidinecarboxamide

HRID 279804
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HRID 279804 반응식
[O:1]=[C:2]1[C@@H:5]([NH:6][C:7](=[O:16])[O:8][CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:4][NH:3]1.C([Li])(CC)C.C1CCCCC1.[CH3:28][S:29]([N:32]=[C:33]=[O:34])(=[O:31])=[O:30].P([O-])([O-])([O-])=O.[K+].[K+].[K+]>O1CCCC1.C(OCC)(=O)C>[CH3:28][S:29]([NH:32][C:33]([N:3]1[CH2:4][C@H:5]([NH:6][C:7]([O:8][CH2:9][C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)=[O:16])[C:2]1=[O:1])=[O:34])(=[O:31])=[O:30]
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참가 물질

8

반응물 5

HCID 8078CyclohexaneHCID 62657Potassium Phosphate, TribasicHCID 12668338Methanesulfonyl isocyanateHCID 12834624benzyl N-[(3S)-2-oxoazetidin-3-yl]carbamateHCID 178418400CID 53628100

생성물 1

HCID 53997697(S)-N-(Methylsulfonyl)-2-oxo-3-[[(phenylmethoxy)-carbonyl]amino]-1-azetidinecarboxamide
수율 53.8%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

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온도
-75 °C

실험 절차

A stirred suspension of (S)-(2-oxo-3-azetidinyl)carbamic acid, phenylmethyl ester (2.20 g; see example 1C) in 60 ml of dry tetrahydrofuran under nitrogen was warmed using a water bath at 40° C. until solution occurs. The solution was cooled to -75° C., and 7.4 ml of 1.35 M sec-butyl lithium in cyclohexane (10 mmol) was added. After stirring for 2 minutes, (methylsulfonyl) isocyanate (about 1.20 g) was added. This reaction was stirred at -75° C. for 10 minutes and poured into 100 ml of 0.5 M pH 5.5 monobasic potassium phosphate buffer. Ethyl acetate was added, and the pH was adjusted to 7. After several extractions with ethyl acetate, the aqueous layer was covered with ethyl acetate and adjusted to pH 2. Repeated extraction with ethyl acetate gave an acidic extract, which was dried (sodium sulfate) and evaporated to a residue (2.61 g). Chromatography of this residue on 250 g of silicAR CC-4 using dichloromethane and then 1% methanol in dichloromethane provided 1.82 g of product as a residue.

후처리

  1. temperaturewas warmed
  2. customat 40° C.
  3. stirringThis reaction was stirred at -75° C. for 10 minutes
  4. extractionAfter several extractions with ethyl acetate
  5. extractionextraction with ethyl acetate
  6. customgave an acidic extract, which
  7. dry with materialwas dried (sodium sulfate)
  8. customevaporated to a residue (2.61 g)

출처 및 근거

ORD 기록
ord-5d299bf7a4df478b8900ba5e5bf3ea22
출처 데이터셋
uspto-grants-1986_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04587047

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