Acetic Anhydride → HCID 12669250, 화합물

HRID 1737253

반응식

HRID 1737253 반응식
[C:1]([NH:4][C:5]1[CH:9]=[CH:8][S:7][C:6]=1[C:10]([OH:12])=[O:11])(=O)[CH3:2].C([O-])(=O)C.[Na+].C(OC(=O)C)(=O)C>O1CCOCC1>[CH3:2][C:1]1[O:12][C:10](=[O:11])[C:6]2[S:7][CH:8]=[CH:9][C:5]=2[N:4]=1

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 517045Sodium AcetateHCID 28075793-Acetamidothiophene-2-carboxylic acid

생성물 1

HCID 12669250HCID 12669250, 화합물수율 119.4%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To a mixture of 3-acetamidothiophene-2-carboxylic acid (15.1 g, 75.67 mmol) and sodium acetate (6.45 g, 78.6 mmol) in dioxane (200 mL) was added acetic anhydride (71 mL, 75.7 mmol). The reaction was refluxed 2 hours, cooled to ambient temperature and partitioned between chloroform and water. Phases were separated and the aqueous layer was extracted with chloroform. The combined organic phase was washed with water and brine, dried over magnesiuym sulfate and concentrated to leave 15.1 g of 2-methyl-thieno[3,2-d][1,3]oxazin-4-one as a brown oil which slowly solidified.

후처리

  1. temperatureThe reaction was refluxed 2 hours
  2. custompartitioned between chloroform and water
  3. customPhases were separated
  4. extractionthe aqueous layer was extracted with chloroform
  5. washThe combined organic phase was washed with water and brine
  6. dry with materialdried over magnesiuym sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f1a00c7973374f43b165a2830c6b3352
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05962457

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