Hydrochloric Acid → HCID 49780164, 화합물

HRID 929505노트

반응식

HRID 929505 반응식
[F:1][C:2]([F:28])([F:27])[O:3][C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:11](=[O:26])[NH:12][CH:13]2[CH2:18][CH2:17][N:16](C(OC(C)(C)C)=O)[CH2:15][CH2:14]2)=[CH:6][CH:5]=1.Cl>CO>[NH:16]1[CH2:17][CH2:18][CH:13]([NH:12][C:11]([NH:10][C:7]2[CH:8]=[CH:9][C:4]([O:3][C:2]([F:1])([F:27])[F:28])=[CH:5][CH:6]=2)=[O:26])[CH2:14][CH2:15]1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 49780163HCID 49780163, 화합물

생성물 1

HCID 49780164HCID 49780164, 화합물수율 89%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Intermediate 41 (2.02 g, 5.0 mmol) was treated with 1M HCl in methanol (35 mL) and refluxed for 3 hours. The solvent was evaporated and the residue diluted with 1N NaOH. The resulting precipitate was removed by filtration and further dried under high vacuum to give intermediate 42 (1.35 g, 89%) as a white solid: Mp 169-173° C. 1H NMR (500 MHz, DMSO-d6) δ 8.49 (s, 1H), 7.46 (d, J=9.0 Hz, 2H), 7.21 (d, J=8.6 Hz, 2H), 6.15 (d, J=7.7 Hz, 1H), 3.55-3.45 (m, 1H), 2.89 (td, J=12.8, 3.5 Hz, 2H), 2.49-2.45 (m, 2H), 2.13 (s, 1H), 1.74 (dd, J=12.4, 2.4 Hz, 2H), 1.21 (dq, J=11.7, 3.7 Hz, 2H). HRMS calculated for C13H16F3N3O2−H+ 302.1117. found (ESI(−), [M−H]) 302.1114.

후처리

  1. temperaturerefluxed for 3 hours
  2. customThe solvent was evaporated
  3. additionthe residue diluted with 1N NaOH
  4. customThe resulting precipitate was removed by filtration
  5. customfurther dried under high vacuum

출처 및 근거

ORD 기록
ord-995633b882af43ddaa081473af61d784
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09296693B2

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