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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Diphenylphosphinic chloride → (5R,6S)-2-[2-(3-Hydroxyiminopyrrolidin-1-yl)-2-iminoethylthio]-6-[(1R)-1-hydroxyethyl]-1-carbapen-2-em-3-carboxylic acid

HRID 622424
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HRID 622424 반응식
C(N(C(C)C)CC)(C)C.C1(P(Cl)(C2C=CC=CC=2)=O)C=CC=CC=1.[OH:25][C@@H:26]([C@H:28]1[C:48](=[O:49])[N:30]2[CH:31]([C:35]([O:37]CC3C=CC([N+]([O-])=O)=CC=3)=[O:36])[C:32](=O)[CH2:33][C@H:29]12)[CH3:27].Cl.[OH:51][N:52]=[C:53]1[CH2:57][CH2:56][N:55]([C:58](=[NH:61])[CH2:59][SH:60])[CH2:54]1>C(#N)C.CS(C)=O.O1CCCC1.O.P([O-])([O-])([O-])=O.[C].[Pd].CCOCC>[OH:51][N:52]=[C:53]1[CH2:57][CH2:56][N:55]([C:58](=[NH:61])[CH2:59][S:60][C:32]2[CH2:33][C@@H:29]3[C@@H:28]([C@H:26]([OH:25])[CH3:27])[C:48](=[O:49])[N:30]3[C:31]=2[C:35]([OH:37])=[O:36])[CH2:54]1
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참가 물질

12

반응물 4

HCID 73910Diphenylphosphinic chlorideHCID 81531Diisopropylethylamine2회HCID 11198839(4-Nitrophenyl)methyl (5R,6S)-6-((1R)-1-hydroxyethyl)-3,7-dioxo-1-azabicyclo(3.2.0)heptane-2-carboxylateHCID 867424332-(3-Hydroxyiminopyrrolidin-1-yl)-2-iminoethylmercaptan hydrochloride

생성물 1

HCID 88522508
(5R,6S)-2-[2-(3-Hydroxyiminopyrrolidin-1-yl)-2-iminoethylthio]-6-[(1R)-1-hydroxyethyl]-1-carbapen-2-em-3-carboxylic acid
수율 3.9%

시약·촉매·용매 7

HCID 178418390HCID 178418390, 화합물촉매HCID 679Dimethyl Sulfoxide용매HCID 962Water용매HCID 1061Phosphate용매HCID 3283Diethyl Ether용매HCID 6342Acetonitrile용매HCID 8028Tetrahydrofuran용매

실험 절차

0.21 ml of diisopropylethylamine and 0.22 ml of diphenylphosphoryl chloride were added dropwise to an ice-cooled solution of 363 mg of p-nitrobenzyl (5R,6S)-6-[(1R)-1-hydroxyethyl]-2-oxo-1-carbapenam-3-carboxylate in 5 ml of anhydrous acetonitrile, and the solution was stirred for one hour with ice-cooling. A solution of 0.18 ml of diisopropylethylamine and 282 mg of 2-(3-hydroxyiminopyrrolidin-1-yl)-2-iminoethylmercaptan hydrochloride in 3 ml of dimethylsulfoxide was added, and the mixture was then stirred for a further 20 minutes with ice-cooling. The reaction mixture was poured into 100 ml of anhydrous ether, and the solvent was decanted off from the gummy material which formed. This material was dissolved in a mixture of 20 ml of tetrahydrofuran, 7 ml of water and 23 ml of 0.1M phosphate buffer (pH 7.0), and the solution was catalytically hydrogenated at room temperature for 2 hours in the presence of 0.3 g of 10 % palladium-carbon. The product was worked up and purified in the same manner as in Example 2, giving 15 mg of the title compound.

후처리

  1. temperaturecooling
  2. stirringthe mixture was then stirred for a further 20 minutes with ice-
  3. temperaturecooling
  4. customthe solvent was decanted off from the gummy material which
  5. customformed
  6. custompurified in the same manner as in Example 2

출처 및 근거

ORD 기록
ord-51573398b3274c11a4f269dea7fd9a71
출처 데이터셋
uspto-grants-1988_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04771046

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