Sodium Hydroxide → Ibuprofen, Sodium Salt

HRID 1731901ノート

反応式

HRID 1731901 の反応式
[OH-].[Na+:2].[OH:3][C:4]([CH:6]([C:8]1[CH:17]=[CH:16][C:11]([CH2:12][CH:13]([CH3:15])[CH3:14])=[CH:10][CH:9]=1)[CH3:7])=[O:5].[Na]>O>[O-:5][C:4]([CH:6]([C:8]1[CH:9]=[CH:10][C:11]([CH2:12][CH:13]([CH3:14])[CH3:15])=[CH:16][CH:17]=1)[CH3:7])=[O:3].[Na+:2]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 45052535IBUPROFEN SODIUM SALT

生成物 1

HCID 5338317Ibuprofen, Sodium Salt

試薬・触媒・溶媒 1

HCID 962Water溶媒3 回

反応条件

温度
95 °C

実験手順

The chloroester solution prepared in (c) was heated to reflux at 95°-100° C. and 13 kg of 50% sodium hydroxide in water was added over twenty minutes. The mixture was refluxed for forty minutes at 95±5° C. GLC analysis of an aliquot indicated complete reaction. 6.4 liters of water were slowly added to the mixture, keeping the temperature about 75° C. After water addition was complete, the mixture was cooled to 70° C. and was seeded with 30 g of good quality sodium ibuprofen. The resulting slurry was cooled to 0° C. over two hours. The slurry was stirred at 0° C. for thirty minutes and filtered. The sodium ibuprofen cake was washed wih 60 kg of heptane and dried.

後処理

  1. temperaturewas heated
  2. temperatureto reflux at 95°-100° C.
  3. customreaction
  4. customthe temperature about 75° C
  5. temperaturethe mixture was cooled to 70° C.
  6. temperatureThe resulting slurry was cooled to 0° C. over two hours
  7. filtrationfiltered
  8. washThe sodium ibuprofen cake was washed wih 60 kg of heptane
  9. customdried

出典と根拠

ORDレコード
ord-e252033bf9fb4d2e8e242cca3d0ce01d
出典データセット
uspto-grants-1986_11
特許番号
US04623736

反応ノート

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