Trifluoromethanesulfonic acid → 8-Isopropyl-6-oxo-5,6-dihydro-4H-2,5,10b-triaza-benzo[e]azulene-3-carboxylic Acid Ethyl Ester

HRID 351839노트

반응식

HRID 351839 반응식
[CH2:1]([O:3][C:4]([C:6]1[N:7]=[CH:8][N:9]2[C:15]=1[CH2:14][N:13](CC1C=CC(OC)=CC=1OC)[C:12](=[O:27])[C:11]1[CH:28]=[C:29]([CH:32]([CH3:34])[CH3:33])[CH:30]=[CH:31][C:10]2=1)=[O:5])[CH3:2].FC(F)(F)S(O)(=O)=O>C(Cl)Cl.FC(F)(F)C(O)=O>[CH2:1]([O:3][C:4]([C:6]1[N:7]=[CH:8][N:9]2[C:15]=1[CH2:14][NH:13][C:12](=[O:27])[C:11]1[CH:28]=[C:29]([CH:32]([CH3:33])[CH3:34])[CH:30]=[CH:31][C:10]2=1)=[O:5])[CH3:2]

참가 물질

5

반응물 2

HCID 62406Trifluoromethanesulfonic acidHCID 699231145-(2,4-Dimethoxy-benzyl)-8-isopropyl-6-oxo-5,6-dihydro-4H-2,5,10b-triaza-benzo[e]azulene-3-carboxylic Acid Ethyl Ester

생성물 1

HCID 699215768-Isopropyl-6-oxo-5,6-dihydro-4H-2,5,10b-triaza-benzo[e]azulene-3-carboxylic Acid Ethyl Ester

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid용매

실험 절차

5-(2,4-Dimethoxy-benzyl)-8-isopropyl-6-oxo-5,6-dihydro-4H-2,5,10b-triaza-benzo[e]azulene-3-carboxylic acid ethyl ester (410 mg, 0.9 mmol) was suspended in CH2Cl2 (3.0 mL), cooled in ice, and diluted slowly with trifluoroacetic acid (2.0 mL). The resulting solution was treated at 5° C. with trifluoromethanesulfonic acid (1.0 mL, 1.3 mmol). The red solution was stirred at room temperature for 2 h. The mixture was then evaporated and dissolved in CH2Cl2 (20 mL), washed with sodium hydrogen carbonate (10%, 2×5 mL) and the organic layer was dried (Na2SO4) and evaporated. Trituration with EtOAc. Yield: 250 mg (90%). m/z 313 (MH).

후처리

  1. temperaturecooled in ice
  2. customThe mixture was then evaporated
  3. dissolutiondissolved in CH2Cl2 (20 mL)
  4. washwashed with sodium hydrogen carbonate (10%, 2×5 mL)
  5. dry with materialthe organic layer was dried (Na2SO4)
  6. customevaporated

출처 및 근거

ORD 기록
ord-6c820a6355104183b83d2eb490d9a0d3
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06743789B2

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