Sodium Hydroxide → HCID 178488147、化合物

HRID 453672

反応式

HRID 453672 の反応式
[CH3:1][C:2]1[CH:3]=[N:4][C:5]([CH2:11][S+:12]([O-:24])[C:13]2[NH:14][C:15]3[CH:16]=[CH:17][C:18]([O:22][CH3:23])=[CH:19][C:20]=3[N:21]=2)=[C:6]([CH3:10])[C:7]=1[O:8][CH3:9].C1C=CC2C(C3C(O)=CC=C4C=3C=CC=C4)=C(O)C=CC=2C=1.[OH-].[Na+]>C(OC)(C)(C)C>[CH3:1][C:2]1[CH:3]=[N:4][C:5]([CH2:11][S+:12]([O-:24])[C:13]2[NH:14][C:15]3[CH:16]=[CH:17][C:18]([O:22][CH3:23])=[CH:19][C:20]=3[N:21]=2)=[C:6]([CH3:10])[C:7]=1[O:8][CH3:9]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 178488158Esomeprazole BINOL

生成物 1

HCID 178488147HCID 178488147、化合物

試薬・触媒・溶媒 1

HCID 15413tert-Butyl methyl ether溶媒

実験手順

Esomeprazole-BINOL inclusion complex (100 g; 158.29 mmol; ee of 98.28%) was suspended in methyl t-butyl ether (1300 ml). Aqueous sodium hydroxide solution (2.2% w/w; 302 g) was added to the suspended mass at 20-30° C. and stirred till clear solution was obtained. Thereafter, organic layer was separated and the aqueous layer was extracted with methyl t-butyl ether for recovery of BINOL. The organic layers were combined, concentrated and recovered 44.4 g of BINOL. To the aqueous layer, methylene chloride (300 ml) was added and pH was adjusted to 7-8 with 10% v/v aqueous acetic acid. The organic layer was separated and washed with DM water and concentrated under reduced pressure to yield esomeprazole as a foamy solid mass.

後処理

  1. customwas obtained
  2. customThereafter, organic layer was separated
  3. extractionthe aqueous layer was extracted with methyl t-butyl ether for recovery of BINOL
  4. concentrationconcentrated
  5. customrecovered 44.4 g of BINOL
  6. additionTo the aqueous layer, methylene chloride (300 ml) was added
  7. customThe organic layer was separated
  8. washwashed with DM water
  9. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-cde4a1f00bf740c79c04cb230bec1eb0
出典データセット
uspto-grants-2013_07
特許番号
US08492551B2

関連ノート

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