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

HRID 1290379노트

반응식

HRID 1290379 반응식
[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]

참가 물질

6

반응물 2

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

생성물 1

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

시약·촉매·용매 3

HCID 23994Zinc촉매HCID 176Acetic Acid용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-f1f04a93c9ea469b846a3df3053b659a
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05750735

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