Acetic Anhydride → Ethanethioic acid trans-(+/-)-S-[5-[[Acetyl(phenylmethoxy)amino]methyl]tetrahydro-3-furanyl]ester

HRID 1290379ノート

反応式

HRID 1290379 の反応式
[C:1]1([CH2:7][O:8][N:9]([CH2:18][C@@H:19]2[O:23][CH2:22][C@@H:21]([S:24][C:25](=[O:27])[CH3:26])[CH2:20]2)[C:10](OCC(Cl)(Cl)Cl)=[O:11])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:28](OC(=O)C)(=O)C>C(O)(=O)C.C(OCC)(=O)C.[Zn]>[C:10]([N:9]([CH2:18][C@@H:19]1[O:23][CH2:22][C@@H:21]([S:24][C:25](=[O:27])[CH3:26])[CH2:20]1)[O:8][CH2:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)(=[O:11])[CH3:28]

参加物

6

反応物 2

HCID 7918Acetic AnhydrideHCID 86752473Ethanethioic acid trans-(+/-)-S-[tetrahydro-5-[[(phenylmethoxy)[(2,2,2-trichloroethoxy)carbonyl]amino]methyl]-3-furanyl] ester

生成物 1

HCID 86750754Ethanethioic acid trans-(+/-)-S-[5-[[Acetyl(phenylmethoxy)amino]methyl]tetrahydro-3-furanyl]ester

試薬・触媒・溶媒 3

HCID 23994Zinc触媒HCID 176Acetic Acid溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a room temperature solution, under argon, of 0.188 g of product from Example 71 in 2.3 ml of glacial acetic acid is added 0.269 g of zinc dust. The reaction is stirred 10 minutes and 155 microliter of acetic anhydride is added. The reaction is stirred at room temperature overnight, diluted with ethyl acetate and filtered. The filtrate is concentrated in vacuo to give 0.110 g of the desired product.

後処理

  1. stirringThe reaction is stirred at room temperature overnight
  2. filtrationfiltered
  3. concentrationThe filtrate is concentrated in vacuo

出典と根拠

ORDレコード
ord-f1f04a93c9ea469b846a3df3053b659a
出典データセット
uspto-grants-1998_05
特許番号
US05750735

反応ノート

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