Trifluoroacetic acid → HCID 178421651, 화합물

HRID 853626노트

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HRID 853626 반응식
[F:1][C:2]1[CH:37]=[CH:36][C:5]([CH2:6][N:7]2[C:19](=[O:20])[C:18]3[C:17]([O:21][Si](C(C)C)(C(C)C)C(C)C)=[C:16]4[C:11]([CH:12]=[CH:13][CH:14]=[N:15]4)=[C:10]([O:32][CH3:33])[C:9]=3[C:8]2(O)[CH3:34])=[CH:4][CH:3]=1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][N:7]2[C:19](=[O:20])[C:18]3[C:17]([OH:21])=[C:16]4[C:11]([CH:12]=[CH:13][CH:14]=[N:15]4)=[C:10]([O:32][CH3:33])[C:9]=3[C:8]2=[CH2:34])=[CH:36][CH:37]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 589289857-(4-Fluoro-benzyl)-6-hydroxy-5-methoxy-6-methyl-9-triisopropylsilanyloxy-6,7-dihydro-pyrrolo[3,4-g]quinolin-8-one

생성물 1

HCID 178421651HCID 178421651, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 16 (10 mg, 0.019 mmol) in 3 mL of CH2Cl2 and TFA (30 μL, 0.389 mmol) was aged for 18 hours. Analysis of the reaction demonstrated complete conversion of starting materials to the product. The solvents were removed under reduced pressure. The residue was dissolved in EtOAc and precipitated with hexanes. The mother liquor was removed and the solid residue was washed with hexanes and subsequently with Et2O to yield the product 17 as a solid. 1H NMR (300 MHz, CDCl3) δ 3.97 (s, 3H), 4.99 (s, 2H), 5.04 (d, 1H, J=2 Hz), 5.63 (d, 1H, J=2 Hz), 6.90 (br s, 1H), 7.04 (t, 2H, J=8 Hz), 7.31 (dd, 2H, J=5, 8 Hz), 7.71 (dd, 1H, J=4, 8 Hz), 8.64 (dd, 1H, J=2, 9 Hz), 9.11 (d, 1H J=3Hz); 19F NMR (282.6 MHz, CDCl3) δ 62.1; EI MS (m/z) 351.5 [MH+], 383.3 [M+Na].

후처리

  1. customThe solvents were removed under reduced pressure
  2. dissolutionThe residue was dissolved in EtOAc
  3. customprecipitated with hexanes
  4. customThe mother liquor was removed
  5. washthe solid residue was washed with hexanes and subsequently with Et2O

출처 및 근거

ORD 기록
ord-5589f1be82974a6b821cb3f468db34af
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07253180B2

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