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Hydrochloric Acid → HCID 71238203, 화합물

HRID 2038719
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HRID 2038719 반응식
[CH2:1]([C:3]1[CH:8]=[C:7]([O:9][CH3:10])[C:6]([F:11])=[CH:5][C:4]=1[C:12]1[CH:20]=[C:19]2[C:15]([CH:16]=[N:17][N:18]2C2CCCCO2)=[CH:14][CH:13]=1)[CH3:2].Cl>CO>[CH2:1]([C:3]1[CH:8]=[C:7]([O:9][CH3:10])[C:6]([F:11])=[CH:5][C:4]=1[C:12]1[CH:20]=[C:19]2[C:15]([CH:16]=[N:17][NH:18]2)=[CH:14][CH:13]=1)[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 712379806-(2-Ethyl-5-fluoro-4-methoxy-phenyl)-1-(tetrahydro-pyran-2-yl)-1H-indazole

생성물 1

HCID 71238203HCID 71238203, 화합물수율 106.9%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
60 °C

실험 절차

To a solution of 6-(2-ethyl-5-fluoro-4-methoxy-phenyl)-1-(tetrahydro-pyran-2-yl)-1H-indazole (Preparation 14, 1.8 g, 5.07 mmol) in methanol (100 mL) was added concentrated hydrochloric acid (12M) and the resulting solution was heated at 60° C. overnight, cooled to room temperature and concentrated in vacuo. The residue was redissolved in EtOAc (50 mL) and washed with saturated sodium hydrogen carbonate aqueous solution (50 mL). The organic layer was dried over MgSO4 and concentrated in vacuo to yield the title product (1.465 g) in 95% yield.

후처리

  1. temperaturecooled to room temperature
  2. concentrationconcentrated in vacuo
  3. dissolutionThe residue was redissolved in EtOAc (50 mL)
  4. washwashed with saturated sodium hydrogen carbonate aqueous solution (50 mL)
  5. dry with materialThe organic layer was dried over MgSO4
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-2122d28368344ea8b43ff1794bf593fe
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08575336B2

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