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Chlorotrimethylsilane → 7-[[(1-Acetyl-4-hydroxy-2-pyrrolidinyl)carbonyl]amino]-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid

HRID 851006
ノート
印刷プレビュー

反応式

HRID 851006 の反応式
[C:1]([N:4]1[CH2:11][CH:10]([OH:12])[CH2:9][C@H:5]1[C:6]([OH:8])=O)(=[O:3])[CH3:2].CN1CCOCC1.ClC(OC)=O.[NH2:25][C:26]1[CH:35]=[C:34]2[C:29]([C:30](=[O:39])[C:31]([C:36]([OH:38])=[O:37])=[CH:32][NH:33]2)=[CH:28][CH:27]=1.C(N(CC)CC)C.Cl[Si](C)(C)C>ClCCl>[C:1]([N:4]1[CH2:11][CH:10]([OH:12])[CH2:9][CH:5]1[C:6]([NH:25][C:26]1[CH:35]=[C:34]2[C:29]([C:30](=[O:39])[C:31]([C:36]([OH:38])=[O:37])=[CH:32][NH:33]2)=[CH:28][CH:27]=1)=[O:8])(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 6

HCID 6397ChlorotrimethylsilaneHCID 6586Methyl chloroformateHCID 79724-MethylmorpholineHCID 8471TriethylamineHCID 2729005(2S)-1-acetyl-4-hydroxypyrrolidine-2-carboxylic acidHCID 102623227-Amino-4-hydroxyquinoline-3-carboxylic acid

生成物 1

HCID 20503439
7-[[(1-Acetyl-4-hydroxy-2-pyrrolidinyl)carbonyl]amino]-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid
収率 73.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A mixture of 6.41 g (37 mmol) of N-acetyl-4-hydroxy-L-proline, 4.07 ml (37 mmol) of N-methyl morpholine, 2.87 ml (37 mmol) of methyl chloroformate, and 90 ml of dichloromethane is stirred at -10° to -20° for 30 minutes. A mixture of 4.08 g (20 mmol) of 7-amino-1, 4-dihydro-4-oxo-3-quinolinecarboxylic acid, 8.4 ml (60 mmol) of triethylamine, 7.6 ml (60 mmol) of chlorotrimethylsilane, and 100 ml of dichloromethane is stirred at room temperature for 30 minutes and then is cooled to -30°. The cold mixed anhydride is added to the cold silylated quinoline and is stirred with cooling for 4 hours and overnight at room temperature. The reaction mixture is evaporated to dryness and the residue is treated with water and 1 N hydrochloric acid. The solid is filtered to give 5.30 g of 7-[[(1-acetyl-4-hydroxy-2-pyrrolidinyl)carbonyl]amino]-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid.

後処理

  1. stirringis stirred at room temperature for 30 minutes
  2. temperatureis cooled to -30°
  3. stirringis stirred
  4. customThe reaction mixture is evaporated to dryness
  5. additionthe residue is treated with water and 1 N hydrochloric acid
  6. filtrationThe solid is filtered

出典と根拠

ORDレコード
ord-c1a3671b4810440c8520bc1197997e17
出典データセット
uspto-grants-1983_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04382089

反応ノート

読み込み中…

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