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Diphenylphosphinic chloride → (5R,6S)-2-{2-[(3R)-3-Carbamoyloxypyrrolidin-1-yl]-2-iminoethylthio}-6-[(1R)-1-hydroxyethyl]-1-carbapen-2-em-3-carboxylic acid

HRID 622412
ノート
印刷プレビュー

反応式

HRID 622412 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.[C:51]([O:54][C@@H:55]1[CH2:59][CH2:58][N:57]([C:60](=[NH:63])[CH2:61][SH:62])[CH2:56]1)(=[O:53])[NH2:52]>C(#N)C.CS(C)=O.O1CCCC1.P([O-])([O-])([O-])=O.[C].[Pd].CCOCC>[C:51]([O:54][C@@H:55]1[CH2:59][CH2:58][N:57]([C:60](=[NH:63])[CH2:61][S:62][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])[CH2:56]1)(=[O:53])[NH2:52]
参加物実験手順後処理出典と根拠反応ノート

参加物

11

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 867424262-[(3R)-3-carbamoyloxypyrrolidin-1-yl]-2-iminoethylmercaptan hydrochloride

生成物 1

HCID 22839799
(5R,6S)-2-{2-[(3R)-3-Carbamoyloxypyrrolidin-1-yl]-2-iminoethylthio}-6-[(1R)-1-hydroxyethyl]-1-carbapen-2-em-3-carboxylic acid
収率 17.6%

試薬・触媒・溶媒 6

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

実験手順

0.183 ml of diisopropylethylamine and 0.218 ml of diphenylphosphoryl chloride were added dropwise to an ice-cooled solution of 348 mg of p-nitrobenzyl (5R,6S)-6-[(1R)-1-hydroxyethyl]-2-oxo-1-carbapenam-3-carboxylate in 5 ml of anhydrous acetonitrile, and the mixture was stirred for 60 minutes with ice-cooling. A solution of 0.183 ml of diisopropylethylamine and 380 mg of 2-[(3R)-3-carbamoyloxypyrrolidin-1-yl]-2-iminoethylmercaptan hydrochloride in 2.5 ml of dimethylsulfoxide was then added dropwise, and the resulting mixture was stirred for a further 30 minutes with ice-cooling. The reaction mixture was poured into 200 ml of anhydrous ether, and the solvent was decanted off from the gummy material which formed. This material was dissolved in a mixture of 35 ml of tetrahydrofuran and 35 ml of 0.1M phosphate buffer (pH 7.0), and the solution was subjected to catalytic hydrogenation for 3 hours at room temperature in the presence of 0.55 g of 10% palladium-carbon. The hydrogenated solution was filtered over "Celite" (Trade Mark) filter aid, and the filtrate was extracted with 80 ml of ether. The aqueous layer was concentrated under reduced pressure, and the concentrate was subjected to chromatography through a 160 ml of column of "Dowex 50W" (Trade Mark) cation exchange resin (Na+ type), giving 70 mg of the title product from the fraction eluted with water.

後処理

  1. temperaturecooling
  2. stirringthe resulting mixture was stirred for a further 30 minutes with ice-
  3. temperaturecooling
  4. customthe solvent was decanted off from the gummy material which
  5. customformed
  6. filtrationThe hydrogenated solution was filtered over "Celite" (Trade Mark)
  7. filtrationfilter aid
  8. extractionthe filtrate was extracted with 80 ml of ether
  9. concentrationThe aqueous layer was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-f454963437c146f187095cf0c53c0dea
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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