Trifluoroacetic acid → HCID 59456972, 화합물

HRID 1711850노트

반응식

HRID 1711850 반응식
C([O:5][C:6](=[O:21])/[CH:7]=[CH:8]/[C:9]1[CH:20]=[N:19][C:12]2[NH:13][C:14](=[O:18])[NH:15][C:16](=[O:17])[C:11]=2[CH:10]=1)(C)(C)C.FC(F)(F)C(O)=O>C(Cl)Cl>[O:18]=[C:14]1[NH:13][C:12]2[N:19]=[CH:20][C:9](/[CH:8]=[CH:7]/[C:6]([OH:21])=[O:5])=[CH:10][C:11]=2[C:16](=[O:17])[NH:15]1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 59456936HCID 59456936, 화합물

생성물 1

HCID 59456972HCID 59456972, 화합물수율 116.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a suspension of (E)-3-(2,4-dioxo-1,2,3,4-tetrahydro-pyrido[2,3-d]pyrimidin-6-yl)acrylic acid tert-butyl ester (379 mg, 1.19 mmol) in CH2Cl2 (10 mL) was added trifluoroacetic acid (2 mL). After 6 h, the solvent was concentrated, the resulting solid was treated with anhydrous HCl (10 mL of a 4 M solution in dioxane, 40 mmol) and the mixture was sonicated for 10 min. The mixture was diluted with Et2O and the solution was filtered. The olive solid was dried under high vacuum at 45° C. overnight to give the title compound (323 mg, 91%) as the TFA salt: 1H NMR (300 MHz, DMSO-d6) δ 11.89 (s, 1H), 11.56 (s, 1H), 8.94 (d, J=1.8 Hz, 1H), 8.53 (d, J=1.8 Hz, 1H), 7.69 (d, J=16.1 Hz, 1H), 6.72 (d, J=16.1 Hz, 1H), 4.40 (bs, 1H); ESI MS m/e 234 (C10H7N3O4+H)+.

후처리

  1. concentrationthe solvent was concentrated
  2. additionthe resulting solid was treated with anhydrous HCl (10 mL of a 4 M solution in dioxane, 40 mmol) and the mixture
  3. customwas sonicated for 10 min
  4. additionThe mixture was diluted with Et2O
  5. filtrationthe solution was filtered
  6. customThe olive solid was dried under high vacuum at 45° C. overnight

출처 및 근거

ORD 기록
ord-03120392822e4ef5a4488754ac745228
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07790709B2

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