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

HRID 1272283노트

반응식

HRID 1272283 반응식
Cl.[CH3:2][C:3]1([CH3:31])[C:7]([CH3:9])(O)[C:6]2[C:10]([CH3:30])=[C:11]([N:16]3[CH2:21][CH2:20][N:19]([C:22]4[CH:27]=[CH:26][C:25]([O:28][CH3:29])=[CH:24][CH:23]=4)[CH2:18][CH2:17]3)[C:12]([CH3:15])=[C:13]([CH3:14])[C:5]=2[O:4]1>C(#N)C>[CH3:29][O:28][C:25]1[CH:24]=[CH:23][C:22]([N:19]2[CH2:20][CH2:21][N:16]([C:11]3[C:12]([CH3:15])=[C:13]([CH3:14])[C:5]4[O:4][C:3]([CH3:2])([CH3:31])[C:7](=[CH2:9])[C:6]=4[C:10]=3[CH3:30])[CH2:17][CH2:18]2)=[CH:27][CH:26]=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

A solution of 10% hydrochloric acid (5 ml) was added to a solution of 1-(2,2,3,4,6,7-hexamethyl-3-hydroxy-2,3-dihydro-1-benzofuran-5-yl)-4-(4-methoxyphenyl)piperazine (1.70 g, 4.14 mmol) obtained in Reference Example 26 in acetonitrile (15 ml) at room temperature and the mixture was stirred for 6 hours. The resulting mixture was concentrated under reduced pressure, and the residue was made to basic with 10% aqueous potassium carbonate. The aqueous layer was extracted with ethyl acetate. The organic extract was washed with water and saturated aqueous sodium chloride, and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure and the residue was crystallized from ethanol to obtain 1.50 g (yield 92%) of the title compound. mp. 134–136° C.

후처리

  1. concentrationThe resulting mixture was concentrated under reduced pressure
  2. extractionThe aqueous layer was extracted with ethyl acetate
  3. extractionThe organic extract
  4. washwas washed with water and saturated aqueous sodium chloride
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was removed under reduced pressure
  7. customthe residue was crystallized from ethanol

출처 및 근거

ORD 기록
ord-f16357ccae1d470687c2d1756f9a2d5c
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07208495B2

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