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Diphenyl chlorophosphate → Allyl (5R,6S)-2-[(2S,4S)-N-allyloxycarbonyl-2-hydroxymethylpyrrolidin-4-ylthio]-6-[(R)-1-allyloxycarbonyloxyethyl]-1-carbapen-2-em-3-carboxylate

HRID 2371831
ノート
印刷プレビュー

反応式

HRID 2371831 の反応式
[CH2:1]([O:4][C:5]([O:7][C@@H:8]([C@H:10]1[C:23](=[O:24])[N:12]2[C@@H:13]([C:17]([O:19][CH2:20][CH:21]=[CH2:22])=[O:18])[C:14](=O)[CH2:15][C@H:11]12)[CH3:9])=[O:6])[CH:2]=[CH2:3].C(N(CC)C(C)C)(C)C.P(Cl)(OC1C=CC=CC=1)(OC1C=CC=CC=1)=O.[CH2:51]([O:54][C:55]([N:57]1[CH2:61][C@@H:60]([SH:62])[CH2:59][C@H:58]1[CH2:63][OH:64])=[O:56])[CH:52]=[CH2:53]>C(#N)C>[CH2:51]([O:54][C:55]([N:57]1[CH2:61][C@@H:60]([S:62][C:14]2[CH2:15][C@@H:11]3[C@@H:10]([C@H:8]([O:7][C:5]([O:4][CH2:1][CH:2]=[CH2:3])=[O:6])[CH3:9])[C:23](=[O:24])[N:12]3[C:13]=2[C:17]([O:19][CH2:20][CH:21]=[CH2:22])=[O:18])[CH2:59][C@H:58]1[CH2:63][OH:64])=[O:56])[CH:52]=[CH2:53]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 75654Diphenyl chlorophosphateHCID 81531Diisopropylethylamine2 回HCID 22842694(2S,4S)-N-Allyloxycarbonyl-2-hydroxymethyl-4-mercaptopyrrolidineHCID 131717188allyl (3R,5R,6S)-6-[(R)-1-allyloxycarbonyloxyethyl]-2-oxo-1-carbapenam-3-carboxylate

生成物 1

HCID 57034286
Allyl (5R,6S)-2-[(2S,4S)-N-allyloxycarbonyl-2-hydroxymethylpyrrolidin-4-ylthio]-6-[(R)-1-allyloxycarbonyloxyethyl]-1-carbapen-2-em-3-carboxylate
収率 75%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

To a solution of allyl (3R,5R,6S)-6-[(R)-1-allyloxycarbonyloxyethyl]-2-oxo-1-carbapenam-3-carboxylate (1.01 g, 3 mmol) and N,N-diisopropylethylamine (0.73 ml, 4.2 mmol) in acetonitrile (20 ml) was dropwise added diphenyl chlorophosphate (0.75-3.6 mmol) under ice-cooling, and then the mixture stirred for 30 minutes. The reaction mixture under ice-cooling was treated successively with N,N-diisopropylethylamine (0.73 μl, 4.2 mmol) and (2S,4S)-N-allyloxycarbonyl-2-hydroxymethyl-4-mercaptopyrrolidine (780 mg, 3.6 mmol) in acetonitrile (4 ml), stirred for 1 hour, and partitioned between ethyl acetate (60 ml) and water (40 ml). The organic layer was successively washed with saturated aqueous sodium bicarbonate and saturated aqueous sodium chloride, dried over anhydrous sodium sulfate, concentrated, and the residue purified by flash column chromatography on silica gel (Wakogel® C-300, 40 ml, elution with ethyl acetate-hexane 1:1) to afford the title compound (1.20 g, 75% yield).

後処理

  1. temperaturecooling
  2. temperatureThe reaction mixture under ice-cooling
  3. stirringstirred for 1 hour
  4. custompartitioned between ethyl acetate (60 ml) and water (40 ml)
  5. washThe organic layer was successively washed with saturated aqueous sodium bicarbonate and saturated aqueous sodium chloride
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated
  8. customthe residue purified by flash column chromatography on silica gel (Wakogel® C-300, 40 ml, elution with ethyl acetate-hexane 1:1)

出典と根拠

ORDレコード
ord-e8a6b138dfa144ac96d29c0780546b54
出典データセット
uspto-grants-1992_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05095013

反応ノート

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