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Hydrochloric Acid → Pyrido[2,3-d]pyrimidine, 4-[2-[4-(1,1-dimethylethyl)phenyl]ethoxy]-

HRID 1087000
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HRID 1087000 반응식
Cl[C:2]1[C:3]2[CH:11]=[CH:10][CH:9]=[N:8][C:4]=2[N:5]=[CH:6][N:7]=1.[C:12]([C:16]1[CH:21]=[CH:20][C:19]([CH2:22][CH2:23][OH:24])=[CH:18][CH:17]=1)([CH3:15])([CH3:14])[CH3:13].Cl>C1(C)C=CC=CC=1>[C:12]([C:16]1[CH:17]=[CH:18][C:19]([CH2:22][CH2:23][O:24][C:2]2[C:3]3[CH:11]=[CH:10][CH:9]=[N:8][C:4]=3[N:5]=[CH:6][N:7]=2)=[CH:20][CH:21]=1)([CH3:15])([CH3:13])[CH3:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 79410p-tert-Butylphenethyl alcoholHCID 5690394-Chloropyrido[2,3-d]pyrimidine

생성물 1

HCID 178230Pyrido[2,3-d]pyrimidine, 4-[2-[4-(1,1-dimethylethyl)phenyl]ethoxy]-

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture consisting of 1.86 g (0.011 mole) of 4-chloropyrido-[2,3-d]pyrimidine, 2.0 g (0.011 mole) of 2-[4-(t-butyl)phenyl]ethanol, and 40 mL of toluene containing a little HCl gas was stirred at room temperature. The mixture was then cooled, and a yellow solid was collected. This was washed with hexane, then partitioned between 1N NaOH and CH2Cl2. The CH2Cl2 layer was dried over MgSO4, then the solvent was removed under vacuum to leave a yellow solid, which was recrystallized from hexane. Yield 2.5 g. M.P. 77-79° C.

후처리

  1. temperatureThe mixture was then cooled
  2. customa yellow solid was collected
  3. washThis was washed with hexane
  4. custompartitioned between 1N NaOH and CH2Cl2
  5. dry with materialThe CH2Cl2 layer was dried over MgSO4
  6. customthe solvent was removed under vacuum
  7. customto leave a yellow solid, which
  8. customwas recrystallized from hexane

출처 및 근거

ORD 기록
ord-98fc451373354d45bcc6b4478b7890c5
출처 데이터셋
uspto-grants-1991_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05034393

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