Hydrochloric Acid → 1-(4-Methoxyphenyl)-4-(2,2,4,6,7-pentamethyl-3-methylidene-2,3-dihydro-1-benzofuran-5-yl)piperazine

HRID 1850403노트

반응식

HRID 1850403 반응식
Cl.[CH3:2][O:3][C:4]1[CH:9]=[CH:8][C:7]([N:10]2[CH2:15][CH2:14][N:13]([C:16]3[C:17]([CH3:31])=[C:18]([CH3:30])[C:19]4[O:23][C:22]([CH3:25])([CH3:24])[C:21]([CH3:27])(O)[C:20]=4[C:28]=3[CH3:29])[CH2:12][CH2:11]2)=[CH:6][CH:5]=1>C(#N)C>[CH3:2][O:3][C:4]1[CH:5]=[CH:6][C:7]([N:10]2[CH2:15][CH2:14][N:13]([C:16]3[C:17]([CH3:31])=[C:18]([CH3:30])[C:19]4[O:23][C:22]([CH3:24])([CH3:25])[C:21](=[CH2:27])[C:20]=4[C:28]=3[CH3:29])[CH2:12][CH2:11]2)=[CH:8][CH:9]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 229356081-(2,2,3,4,6,7-Hexamethyl-3-hydroxy-2,3-dihydro-1-benzofuran-5-yl)-4-(4-methoxyphenyl)piperazine

생성물 1

HCID 229355751-(4-Methoxyphenyl)-4-(2,2,4,6,7-pentamethyl-3-methylidene-2,3-dihydro-1-benzofuran-5-yl)piperazine수율 92.3%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

10% hydrochloric acid (5 mL) was added to a suspension of acetonitrile (15 mL) containing 5-[4-(4-methoxyphenyl)piperazin-1-yl]-2,2,3,4,6,7-hexamethyl-2,3-dihydro-1-benzofuran-3-ol (1.70 g, 4.14 mmol) obtained in Reference Example 105, and the mixture was stirred at room temperature for 6 hours. The reaction solution was concentrated under reduced pressure, and after that, 10% potassium carbonate aqueous solution was added to the residue so that the aqueous layer became alkaline. Then, extraction was performed using ethyl acetate. The organic layer was washed with water and saturated saline, and then dried using anhydrous sodium sulfate. The solvent was removed under reduced pressure, and the obtained residue was crystallized using ethanol to give 1.50 g of the title compound (yield: 92%)

후처리

  1. customobtained in Reference Example 105
  2. concentrationThe reaction solution was concentrated under reduced pressure
  3. additionafter that, 10% potassium carbonate aqueous solution was added to the residue so that the aqueous layer
  4. extractionThen, extraction
  5. washThe organic layer was washed with water and saturated saline
  6. customdried
  7. customThe solvent was removed under reduced pressure
  8. customthe obtained residue was crystallized

출처 및 근거

ORD 기록
ord-a1b6d9c52aa54d268b5dbf3519bcdc23
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08957069B2

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