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Formic Acid → HCID 14230762、化合物

HRID 465257
ノート
印刷プレビュー

反応式

HRID 465257 の反応式
C([NH:20][C:21]1[S:22][CH:23]=[C:24](/[C:26](=[N:31]/[O:32][CH2:33][CH:34]=[CH2:35])/[C:27]([O:29][CH3:30])=[O:28])[N:25]=1)(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.C(O)=O>O1CCCC1>[NH2:20][C:21]1[S:22][CH:23]=[C:24](/[C:26](=[N:31]/[O:32][CH2:33][CH:34]=[CH2:35])/[C:27]([O:29][CH3:30])=[O:28])[N:25]=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

4

反応物 2

HCID 284Formic AcidHCID 14230767HCID 14230767、化合物

生成物 1

HCID 14230762HCID 14230762、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

In 32 ml of tetrahydrofuran is dissolved 6.45 g of methyl 2-(2-tritylamino-4-thiazolyl)-(Z)-2-allyloxyiminoacetate, followed by addition of 32 ml of 50% formic acid. The mixture is stirred at 60° C. for 40 minutes. The reaction mixture is concentrated under reduced pressure and the solid residue is dissolved in ethyl acetate, washed with aqueous sodium hydrogen carbonate and aqueous sodium chloride in this order, and dried over anhydrous sodium sulfate. The solvent is then distilled off under reduced pressure and the residue is purified by column chromatography [silica gel: 150 g; eluent: hexane-ethyl acetate (1:1)]. The solvent is distilled off and the solid residue is washed with hexane and a small amount of ether in this order, and then dried to give methyl 2-(2-amino-4-thiazolyl)-(Z)-2-allyloxyiminoacetate, m.p. 133°-134° C.

後処理

  1. concentrationThe reaction mixture is concentrated under reduced pressure
  2. dissolutionthe solid residue is dissolved in ethyl acetate
  3. washwashed with aqueous sodium hydrogen carbonate and aqueous sodium chloride in this order
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationThe solvent is then distilled off under reduced pressure
  6. customthe residue is purified by column chromatography [silica gel: 150 g; eluent: hexane-ethyl acetate (1:1)]
  7. distillationThe solvent is distilled off
  8. washthe solid residue is washed with hexane
  9. dry with materiala small amount of ether in this order, and then dried

出典と根拠

ORDレコード
ord-603b303fc16c4db4820a86c1e727d9bc
出典データセット
uspto-grants-1985_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04550105

反応ノート

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