Acetic Anhydride → HCID 12669250, 화합물

HRID 430508

반응식

HRID 430508 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-82c2df153c004ea5b5d5c17398b9629d
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06323208B1

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