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Potassium Carbonate → Propyl 2-(2-methoxyphenyl)-3-phenyl-2-[(1,2,4-triazol-1-yl)methyl]-propionate

HRID 257735
ノート
印刷プレビュー

反応式

HRID 257735 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]([CH2:20][N:21]1[CH:25]=[N:24][CH:23]=[N:22]1)([CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:10]([OH:12])=[O:11].C(=O)([O-])[O-].[K+].[K+].I[CH2:33][CH2:34][CH3:35]>C(C(C)=O)C>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]([CH2:20][N:21]1[CH:25]=[N:24][CH:23]=[N:22]1)([CH2:13][C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1)[C:10]([O:12][CH2:33][CH2:34][CH3:35])=[O:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 336431-IodopropaneHCID 200852002-(2-Methoxyphenyl)-3-phenyl-2-[(1,2,4-triazol-1-yl)methyl]propanoic acid

生成物 1

HCID 20085202Propyl 2-(2-methoxyphenyl)-3-phenyl-2-[(1,2,4-triazol-1-yl)methyl]-propionate収率 82%

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

A mixture of 2-(2-methoxyphenyl)-3-phenyl-2-[(1,2,4-triazol-1-yl)methyl]propanoic acid (6.0 g, 0.0178 mole) and potassium carbonate (3.6 g, 0.0213 mole) in methyl ethyl ketone (50 mL) was stirred and heated to reflux for 1 hour. Iodopropane (3.6 g, 0.0213 mole) was added and the mixture continued heating at reflux for an additional 4 hours and then allowed to cool to room temperature. The solvent was removed by distillation and 100 mL of water and 100 mL of ethyl acetate added. The organic phase was then separated, dried and concentrated on a rotary evaporator to afford 5.5 g of solid product (melting point 129°-130° C.; yield 82%), Example 100 of Table 1.

後処理

  1. temperatureheated
  2. temperatureto reflux for 1 hour
  3. temperaturethe mixture continued heating
  4. temperatureat reflux for an additional 4 hours
  5. customThe solvent was removed by distillation and 100 mL of water and 100 mL of ethyl acetate
  6. additionadded
  7. customThe organic phase was then separated
  8. customdried
  9. concentrationconcentrated on a rotary evaporator

出典と根拠

ORDレコード
ord-b1b80f95c8624ba180cea41f85df0650
出典データセット
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05264415

反応ノート

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