Trifluoroacetic acid → HCID 21269512, 화합물

HRID 2231509노트

반응식

HRID 2231509 반응식
O.Br.[OH:3][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][C:13]=1[OH:14])[CH:10]=[N:9][CH:8]=[CH:7]2.[C:15](OC(=O)C)(=[O:17])[CH3:16].F[C:23](F)(F)[C:24](O)=[O:25]>>[C:15]([O:3][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][C:13]=1[O:14][C:24](=[O:25])[CH3:23])[CH:10]=[N:9][CH:8]=[CH:7]2)(=[O:17])[CH3:16]

참가 물질

4

반응물 3

HCID 6422Trifluoroacetic acidHCID 7918Acetic AnhydrideHCID 135574541HCID 135574541, 화합물

생성물 1

HCID 21269512HCID 21269512, 화합물수율 93.4%

실험 절차

500 mg (1.9 mmol) of 6,7-dihydroxyisoquinoline hydrobromide monohydrate was suspended in 10 ml of trifluoroacetic acid, and 2.0 ml (21 mmol) of acetic anhydride was added thereto at room temperature. The mixture was stirred at the same temperature for 24 hours. The reaction solution was concentrated under reduced pressure. Water and ethyl acetate were added to the residue. Then, the aqueous solution was adjusted to pH 8.0 with a 5% sodium hydrogen carbonate aqueous solution, and extracted with ethyl acetate. The extract was washed with a saturated sodium chloride aqueous solution, then dried over anhydrous sodium sulfate and concentrated under reduced pressure to obtain 440 mg (yield: 93.4%) of the above identified compound.

후처리

  1. customat room temperature
  2. concentrationThe reaction solution was concentrated under reduced pressure
  3. additionWater and ethyl acetate were added to the residue
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with a saturated sodium chloride aqueous solution
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customto obtain 440 mg (yield: 93.4%) of the

출처 및 근거

ORD 기록
ord-b879cfca5551415b8a402f4be4ed4b4c
출처 데이터셋
uspto-grants-1988_11
특허 번호
US04782155

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