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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
ノート
印刷プレビュー

反応式

HRID 622424 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

12

反応物 4

HCID 73910Diphenylphosphinic chlorideHCID 81531Diisopropylethylamine2 回HCID 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

生成物 1

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

試薬・触媒・溶媒 7

HCID 178418390HCID 178418390、化合物触媒HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒HCID 1061Phosphate溶媒HCID 3283Diethyl Ether溶媒HCID 6342Acetonitrile溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-51573398b3274c11a4f269dea7fd9a71
出典データセット
uspto-grants-1988_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04771046

反応ノート

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