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Pyridine → ethyl (E)-6-(1,3-dihydro-4-carbamoyloxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate

HRID 4413
ノート
印刷プレビュー

反応式

HRID 4413 の反応式
[OH:1][C:2]1[C:10]([CH2:11]/[CH:12]=[C:13](\[CH3:21])/[CH2:14][CH2:15][C:16]([O:18][CH2:19][CH3:20])=[S:17])=[C:9]([O:22][CH3:23])[C:8]([CH3:24])=[C:7]2[C:3]=1[C:4](=[O:25])[O:5][CH2:6]2.[N:26]1[CH:31]=CC=CC=1.C(Cl)(Cl)=[O:33]>C1C=CC=CC=1>[C:31]([O:1][C:2]1[C:10]([CH2:11]/[CH:12]=[C:13](\[CH3:21])/[CH2:14][CH2:15][C:16]([O:18][CH2:19][CH3:20])=[S:17])=[C:9]([O:22][CH3:23])[C:8]([CH3:24])=[C:7]2[C:3]=1[C:4](=[O:25])[O:5][CH2:6]2)(=[O:33])[NH2:26]
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

5

反応物 3

HCID 1049PyridineHCID 6371PhosgeneHCID 86741995HCID 86741995、化合物

生成物 1

HCID 86741994ethyl (E)-6-(1,3-dihydro-4-carbamoyloxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

反応条件

温度
25 °C

実験手順

To a solution of 500 mgs of ethyl (E)-6-(1,3-dihydro-4-hydroxy-6-methoxy-7-methyl-3-oxo-5-isobenzofuranyl)-4-methyl-4-thiohexenoate in 10 ml of benzene cooled in an ice bath was added 0.1 ml of pyridine and 6 ml of a 12.5% solution of phosgene in benzene. The solution was stirred at 25° C. overnight, the precipitate filtered off and solvent removed from the filtrate under reduced pressure. The residue was dissolved in 5 ml of tetrahydrofuran and to this solution was added dropwise a solution of ammonia in tetrahydrofuran until the reaction was complete. The mixture was poured into water and extracted with ethyl acetate. The organic solution was dried over magnesium sulfate and evaporated to an oil which was chromatographed on silica gel, eluting with a 1:1 mixture of ethyl acetate and hexane. The purified product was stirred with a mixture of ether and hexane and filtered giving ethyl (E)-6-(1,3-dihydro-4-carbamoyl oxy-6-methoxy-7-methyl-3-oxo-5-iso benzofuranyl)-4-methyl-4-thiohexenoate, mp 145°-147° C.

後処理

  1. filtrationthe precipitate filtered off
  2. customsolvent removed from the filtrate under reduced pressure
  3. dissolutionThe residue was dissolved in 5 ml of tetrahydrofuran and to this solution
  4. additionwas added dropwise a solution of ammonia in tetrahydrofuran until the reaction
  5. additionThe mixture was poured into water
  6. extractionextracted with ethyl acetate
  7. dry with materialThe organic solution was dried over magnesium sulfate
  8. customevaporated to an oil which
  9. customwas chromatographed on silica gel
  10. washeluting with a 1:1 mixture of ethyl acetate and hexane
  11. stirringThe purified product was stirred with a mixture of ether and hexane
  12. filtrationfiltered

出典と根拠

ORDレコード
ord-af833aac68e84efd9b9b7fe09d4bd9be
出典データセット
uspto-grants-1988_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04725622

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート