Trifluoroacetic acid → HCID 21269512、化合物

HRID 2231509ノート

反応式

HRID 2231509 の反応式
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]

参加物

4

反応物 3

HCID 6422Trifluoroacetic acidHCID 7918Acetic AnhydrideHCID 135574541HCID 135574541、化合物

生成物 1

HCID 21269512HCID 21269512、化合物収率 93.4%

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b879cfca5551415b8a402f4be4ed4b4c
出典データセット
uspto-grants-1988_11
特許番号
US04782155

反応ノート

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