Hydrochloric Acid → HCID 59383129、化合物

HRID 2355245ノート

反応式

HRID 2355245 の反応式
I([O-])(=O)(=O)=O.[Na+].[C:7]([O:11][C:12]([N:14]1[C:19]([CH3:21])([CH3:20])[CH2:18][CH2:17][O:16][S:15]1=[O:22])=[O:13])([CH3:10])([CH3:9])[CH3:8].P([O-])([O-])(O)=[O:24].[Na+].[Na+].Cl>O.C(#N)C.O.[Ru](Cl)(Cl)Cl>[C:7]([O:11][C:12]([N:14]1[C:19]([CH3:21])([CH3:20])[CH2:18][CH2:17][O:16][S:15]1(=[O:24])=[O:22])=[O:13])([CH3:10])([CH3:8])[CH3:9]

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 24203Sodium Phosphate, Dibasic2 回HCID 23667635Sodium periodateHCID 58875133HCID 58875133、化合物

生成物 1

HCID 59383129HCID 59383129、化合物

試薬・触媒・溶媒 3

HCID 6093376Ruthenium trichloride hydrate触媒HCID 962Water溶媒HCID 6342Acetonitrile溶媒

反応条件

温度
20 °C

実験手順

A solution of ruthenium(III)chloride hydrate (440 mg, 2.12 mmol, 0.003 equiv) and sodium metaperiodate (132.2 g, 0.62 mol) in water (1.5 l) is stirred for 45 min and added at a temperature of 20-25° C. over a period of 35 min to a suspension of the crude product of Step b (140 g) in a mixture of acetonitrile (0.6 l) and saturated aqueous solution of disodium hydrogen phosphate (0.3 l). During the addition the pH of the suspension is kept between 6.9 and 7.3 by the continuous addition of additional saturated aqueous solution of disodium hydrogen phosphate (1.0 l). After the addition has ended the reaction mixture is stirred for 1 hour at 20° C., the pH is adjusted to 6.4 with 1 M hydrochloric acid and then stirring is continued for a further hour. The solid is collected by filtration, washed with water (3×100 ml) and lastly stirred for 2 hours with water (1.5 l). The crystals are isolated by filtration, washed with water (3×0.1 l) and dried at 50° C.

後処理

  1. additionDuring the addition the pH of the suspension
  2. additionAfter the addition
  3. stirringstirring
  4. waitis continued for a further hour
  5. filtrationThe solid is collected by filtration
  6. washwashed with water (3×100 ml)
  7. stirringlastly stirred for 2 hours with water (1.5 l)
  8. customThe crystals are isolated by filtration
  9. washwashed with water (3×0.1 l)
  10. customdried at 50° C.

出典と根拠

ORDレコード
ord-79bf50223e334a0e92486c73feb15891
出典データセット
uspto-grants-2010_07
特許番号
US07754756B2

反応ノート

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