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Carbon Disulfide → p-Nitrobenzyl 2-(4-hydroxy-1,3-dithiolan-2-ylidene)-2-(4-methylthio-2-azetidinon-1-yl)acetate

HRID 980966
ノート
印刷プレビュー

反応式

HRID 980966 の反応式
C([Li])CCC.[CH3:6][S:7][CH:8]1[N:11]([CH2:12][C:13]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][C:20]([N+:23]([O-:25])=[O:24])=[CH:19][CH:18]=2)=[O:14])[C:10](=[O:26])[CH2:9]1.[C:27](=[S:29])=[S:28].I[CH2:31][CH:32]=[O:33]>CCCCCC.O1CCCC1.C(O)(=O)C.C(OCC)(=O)C>[OH:33][CH:32]1[CH2:31][S:29][C:27](=[C:12]([N:11]2[CH:8]([S:7][CH3:6])[CH2:9][C:10]2=[O:26])[C:13]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][C:20]([N+:23]([O-:25])=[O:24])=[CH:19][CH:18]=2)=[O:14])[S:28]1
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

9

反応物 4

HCID 6348Carbon DisulfideHCID 10219603IodoacetaldehydeHCID 20220761p-Nitrobenzyl (4-methylthio-2-azetidinon-1-yl)acetateHCID 178418339Butyllithium

生成物 1

HCID 86741253p-Nitrobenzyl 2-(4-hydroxy-1,3-dithiolan-2-ylidene)-2-(4-methylthio-2-azetidinon-1-yl)acetate

試薬・触媒・溶媒 4

HCID 176
Acetic Acid
溶媒
HCID 8028Tetrahydrofuran溶媒3 回
HCID 8058Hexane溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
-78 °C

実験手順

A solution of butyllithium in hexane (2.4 ml, 1.63 mmoles/ml) was added to a solution of hexamethyldisilazene (740 μl) in tetrahydrofuran (12 ml) at room temperature, and then the mixture was stirred for 30 minutes. The solution was cooled to -78° C. and a solution of p-nitrobenzyl (4-methylthio-2-azetidinon-1-yl)acetate (620 mg) in tetrahydrofuran (5 ml) was added thereto, and the mixture was stirred for 10 minutes. Carbon disulphide (181 μl) was added to the resulting mixture, which was then stirred for 1 hour. A solution of iodoacetaldehyde (503 mg) in tetrahydrofuran was added to the solution, after which the mixture was stirred at -78° C. for 2 hours. The reaction mixture was then diluted with acetic acid (606 μl) and ethyl acetate and washed successively with an aqueous solution of sodium chloride, an aqueous solution of sodium bicarbonate and again an aqueous solution of sodium chloride and dried over anhydrous sodium sulphate. The solvent was distilled off under reduced pressure and the resulting residue was dissolved in tetrahydrofuran (4 ml). A drop of p-toluenesulphonic acid was added to the solution, which was then stirred at room temperature for 1.5 hours. The solvent was distilled off under reduced pressure and the resulting residue was purified by column chromatography (eluent: a 1:1 by volume mixture of benzene and ethyl acetate), to give 733 mg of the desired product as a foamy substance.

後処理

  1. stirringthe mixture was stirred for 10 minutes
  2. stirringwas then stirred for 1 hour
  3. stirringafter which the mixture was stirred at -78° C. for 2 hours
  4. washwashed successively with an aqueous solution of sodium chloride
  5. dry with materialan aqueous solution of sodium bicarbonate and again an aqueous solution of sodium chloride and dried over anhydrous sodium sulphate
  6. distillationThe solvent was distilled off under reduced pressure
  7. dissolutionthe resulting residue was dissolved in tetrahydrofuran (4 ml)
  8. additionA drop of p-toluenesulphonic acid was added to the solution, which
  9. stirringwas then stirred at room temperature for 1.5 hours
  10. distillationThe solvent was distilled off under reduced pressure
  11. customthe resulting residue was purified by column chromatography (eluent
  12. additiona 1:1 by volume mixture of benzene and ethyl acetate),

出典と根拠

ORDレコード
ord-c8652b43724643f19a800a57d17fe79c
出典データセット
uspto-grants-1987_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04639441

反応ノート

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