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

HRID 2063812ノート

反応式

HRID 2063812 の反応式
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

参加物

4

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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%)

後処理

  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

出典と根拠

ORDレコード
ord-a184c4090b73473fa7a648037186c6fc
出典データセット
uspto-grants-2012_10
特許番号
US08288390B2

反応ノート

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