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

HRID 1850430
ノート
印刷プレビュー

反応式

HRID 1850430 の反応式
Br[C:2]1[C:3]([CH3:15])=[C:4]([CH3:14])[C:5]2[O:9][C:8]([CH3:11])([CH3:10])[CH2:7][C:6]=2[C:12]=1[CH3:13].[CH3:16][O:17][C:18]1[CH:23]=[CH:22][C:21]([N:24]2[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]2)=[CH:20][CH:19]=1.C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1.CC(C)([O-])C.[Na+]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.O.C1(C)C=CC=CC=1>[CH3:16][O:17][C:18]1[CH:19]=[CH:20][C:21]([N:24]2[CH2:29][CH2:28][N:27]([C:2]3[C:3]([CH3:15])=[C:4]([CH3:14])[C:5]4[O:9][C:8]([CH3:11])([CH3:10])[CH2:7][C:6]=4[C:12]=3[CH3:13])[CH2:26][CH2:25]2)=[CH:22][CH:23]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 2697221-(4-Methoxyphenyl)piperazine2 回HCID 634876Binap, (A+-)-HCID 23676156Sodium t-butoxideHCID 667609285-Bromo-2,2,4,6,7-pentamethyl-2,3-dihydrobenzofuran2 回

生成物 1

HCID 469103861-(4-Methoxyphenyl)-4-(2,2,4,6,7-pentamethyl-2,3-dihydro-1-benzofuran-5-yl)piperazine収率 20.9%

試薬・触媒・溶媒

3
HCID 167845palladium(II) acetate触媒HCID 962Water溶媒HCID 1140Toluene溶媒

実験手順

In addition, synthesis was also performed according to the below-described method using 5-bromo-2,2,4,6,7-pentamethyl-2,3-dihydro-1-benzofuran (344.1 g, 1.28 mol) synthesized in Reference Example 4 and 1-(4-methoxyphenyl)piperazine (164 g, 853 mmol). That is, 1-(4-methoxyphenyl)piperazine (51.5 g, 268 mmol), palladium acetate (3.01 g, 13.4 mmol), BINAP (12.5 g, 20.1 mmol) and sodium tert-butoxide (38.6 g, 402 mmol) were added to a solution of toluene (775 mL) containing 5-bromo-2,2,4,6,7-pentamethyl-2,3-dihydro-1-benzofuran (108 g, 402 mmol), and the mixture was heated to reflux under argon atmosphere for 7 hours. After cooled to room temperature, water (775 mL) was added to the reaction solution for distribution. The organic layer was washed with saturated saline (515 mL) and dried using anhydrous magnesium sulfate, and after that, the solvent was removed under reduced pressure. The obtained residue was purified by basic silica gel column chromatography (hexane-ethyl acetate 98:2) and then silica gel column chromatography (hexane-ethyl acetate 100:0-94:6) to give a crudely purified product of the title compound as a yellow solid (68.0 g). Similarly, a crudely purified product of the title compound (136.6 g) was obtained from 5-bromo-2,2,4,6,7-pentamethyl-2,3-dihydro-1-benzofuran (213 g, 791 mmol) and 1-(4-methoxyphenyl)piperazine (101.5 g, 528 mmol). The obtained crudely purified products were put together and suspended in ethanol (2.3 L). This suspension was stirred at 65° C. for 30 minutes. After cooled to room temperature, it was further stirred for 1 hour, and crystals were collected by filtration to give a crude crystal of the title compound (181 g). Similarly, a crude crystal of the title compound was obtained from 5-bromo-2,2,4,6,7-pentamethyl-2,3-dihydro-1-benzofuran (23.1 g, 85.8 mmol) and 1-(4-methoxyphenyl)piperazine (11.0 g, 57.2 mmol). The obtained crude crystals were put together and recrystallized from acetone (2.82 L)/water (940 mL) to give 176 g of the title compound as a colorless crystal (yield: 54%). Melting point was 152 to 155° C.

後処理

  1. customIn addition, synthesis
  2. temperaturethe mixture was heated
  3. temperatureto reflux under argon atmosphere for 7 hours
  4. washThe organic layer was washed with saturated saline (515 mL)
  5. customdried
  6. customafter that, the solvent was removed under reduced pressure
  7. customThe obtained residue was purified by basic silica gel column chromatography (hexane-ethyl acetate 98:2)

出典と根拠

ORDレコード
ord-d3ac495d23ff446ab93ce3d9019a29ca
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08957069B2

反応ノート

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