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Phosphate → (1R,5S,6S)-2-[(4R)-pyrrolidine-2-thion-4-ylthio]-6-[(1R)-1-hydroxyethyl]-1-methylcarbapen-2-em-3-carboxylic acid isobutyryloxymethyl ester

HRID 257288
ノート
印刷プレビュー

反応式

HRID 257288 の反応式
[C:1]([O:6][CH2:7][O:8][C:9]([C:11]1[N:15]2[C:16](=[O:28])[C@H:17]([C@H:18]([O:20][Si](C(C)(C)C)(C)C)[CH3:19])[C@H:14]2[C@@H:13]([CH3:29])[C:12]=1[S:30][C@H:31]1[CH2:35][NH:34][C:33](=[S:36])[CH2:32]1)=[O:10])(=[O:5])[CH:2]([CH3:4])[CH3:3].CN(C)C=O.F.[NH4+].P([O-])([O-])([O-])=O>CN1CCCC1=O>[C:1]([O:6][CH2:7][O:8][C:9]([C:11]1[N:15]2[C:16](=[O:28])[C@H:17]([C@H:18]([OH:20])[CH3:19])[C@H:14]2[C@@H:13]([CH3:29])[C:12]=1[S:30][C@H:31]1[CH2:35][NH:34][C:33](=[S:36])[CH2:32]1)=[O:10])(=[O:5])[CH:2]([CH3:3])[CH3:4]
参加物反応条件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 1061PhosphateHCID 6228DimethylformamideHCID 11103665(1R,5S,6S)-2-[(4R)-pyrrolidine-2-thion-4-ylthio]-6-[(1R)-1-t-butyldimethylsilyloxyethyl]-1-methylcarbapen-2-em-3-carboxylic acid isobutyryloxymethyl esterHCID 13685747Ammonium hydrogenfluoride

生成物 1

HCID 9955020
(1R,5S,6S)-2-[(4R)-pyrrolidine-2-thion-4-ylthio]-6-[(1R)-1-hydroxyethyl]-1-methylcarbapen-2-em-3-carboxylic acid isobutyryloxymethyl ester
収率 91%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
20 °C

実験手順

A mixture of (1R,5S,6S)-2-[(4R)-pyrrolidine-2-thion-4-ylthio]-6-[(1R)-1-t-butyldimethylsilyloxyethyl]-1-methylcarbapen-2-em-3-carboxylic acid isobutyryloxymethyl ester (3 g), dimethylformamide (20 ml), N-methylpyrrolidone (7 ml) and ammonium hydrogenfluoride (1.21 g) is stirred at 20° C. for three days. The reaction mixture is poured into a phosphate buffer (pH 7.0), and the mixture is extracted with ethyl acetate. The aqueous layer is extracted with ethyl acetate, and the organic layers are combined, washed with water, dried, and concentrated under reduced pressure. The resulting residue is crystallized from a mixture of ethyl acetate and diisopropyl ether. To the resultant is added diisopropyl ether, and the precipitate is collected by filtration, and washed to give (1R,5S,6S)-2-[(4R)-pyrrolidine-2-thion-4-ylthio]-6-[(1R)-1-hydroxyethyl]-1-methylcarbapen-2-em-3-carboxylic acid isobutyryloxymethyl ester (2.17 g) as crystals.

後処理

  1. extractionthe mixture is extracted with ethyl acetate
  2. extractionThe aqueous layer is extracted with ethyl acetate
  3. washwashed with water
  4. customdried
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting residue is crystallized from a mixture of ethyl acetate and diisopropyl ether
  7. additionTo the resultant is added diisopropyl ether
  8. filtrationthe precipitate is collected by filtration
  9. washwashed

出典と根拠

ORDレコード
ord-d15255eae5ed479dbac0768ff8dfab88
出典データセット
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05260438

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート