Hydrochloric Acid → HCID 178433400, 화합물

HRID 241457노트

반응식

HRID 241457 반응식
[F:1][CH:2]([F:19])[C:3]1[N:8]=[CH:7][C:6]([C:9]2[NH:13][C:12]([NH:14]C(=O)C)=[N:11][C:10]=2[CH3:18])=[CH:5][CH:4]=1.Cl>CO.O>[F:19][CH:2]([F:1])[C:3]1[N:8]=[CH:7][C:6]([C:9]2[NH:13][C:12]([NH2:14])=[N:11][C:10]=2[CH3:18])=[CH:5][CH:4]=1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 178474433HCID 178474433, 화합물

생성물 1

HCID 178433400HCID 178433400, 화합물수율 105%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

Dissolve N-[5-[6-(difluoromethyl)-3-pyridyl]-4-methyl-1H-imidazol-2-yl]acetamide (0.172 g, 0.65 mmol) in MeOH (5 mL) and water (5 mL). Heat the mixture to 60° C. Add hydrochloric acid (12 N, 5 mL, 60 mmol). Stir mixture for 2 hours at 60° C. Concentrate the mixture to a volume of about 10 mL. Adjust the pH of the aqueous solution to 8. Extract the resulting solution with EtOAc (2×20 mL). Dry the combined organic extracts over sodium sulfate; filter; collect the filtrate; and concentrate the filtrate under reduced pressure to give the title compound as a yellow oil (0.153 g, 100% crude yield). LCMS (m/z) 225 (M+1).

후처리

  1. concentrationConcentrate the mixture to a volume of about 10 mL
  2. extractionExtract the resulting solution with EtOAc (2×20 mL)
  3. dry with materialDry the combined organic extracts over sodium sulfate
  4. filtrationfilter
  5. customcollect the filtrate
  6. concentrationand concentrate the filtrate under reduced pressure

출처 및 근거

ORD 기록
ord-680f169aa1f44a10b1c5997d55b30285
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08648200B2

반응 노트

불러오는 중…