Sulfuric Acid → barium L-ascorbate 2-sulfate dihydrate

HRID 1076030

反応式

HRID 1076030 の反応式
[O:1]=[C:2]1[O:8][C@H:7]([C@H:9]([CH2:11][OH:12])[OH:10])[C:5]([OH:6])=[C:3]1[OH:4].O.O.O.O.O.O.O.O.[OH-].[Ba+2:22].[OH-].CN(C)C.S(=O)(=O)=[O:29].C(=O)([O-])[O-].[K+].[K+].[OH-].[Ba+2].[OH-].CN(C)C.[S:45](=O)(=[O:48])([OH:47])[OH:46]>O>[OH2:1].[OH2:29].[S:45]([O:4][C:3]1[C:2]([O:8][C@H:7]([C@H:9]([CH2:11][OH:12])[OH:10])[C:5]=1[O-:6])=[O:1])([O-:48])(=[O:47])=[O:46].[Ba+2:22]

参加物

9

反応物 7

HCID 1118Sulfuric AcidHCID 1146TrimethylamineHCID 11430Potassium CarbonateHCID 222852Methanamine, N,N-dimethyl-, compd. with sulfur trioxide (1:1)HCID 6093286Barium hydroxideHCID 17749109Barium hydroxide, octahydrate3 回HCID 54670067L-Ascorbic Acid

生成物 1

HCID 131710190barium L-ascorbate 2-sulfate dihydrate収率 80%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

To a mixture of water (25.0) and L-ascorbic acid (2.0g, 11.5 millimoles) was added barium hydroxide octahydrate with stirring until the solution had pH 10.5. The mixture was warmed to 70°, and trimethylamine-sulfur trioxide (2.4g, 1.5 equivalent) was added. Solid barium hydroxide octahydrate was added intermittently to maintain the reaction pH at 10.5. A total of 5g of barium hydroxide octahydrate was used in the reaction to this point. After 30 minutes the reaction was complete as indicated by thin-layer chromatography. The mixture was cooled and a saturated aqueous solution of barium hydroxide (1-2 ml) was added to adjust the solution pH to 12.5. Nitrogen was passed through the mixture at 70° to expel trimethylamine. The solution was diluted with water (100 ml) and neutralized with aqueous sulfuric acid. Insoluble barium sulfate was removed by filtration, and the filtrate decolorized with charcoal and evaporated to a small volume (30 ml). Addition of methanol (30 ml) followed by cooling gave 3.94 g (80%) of barium L-ascorbate 2-sulfate dihydrate with m.p. 234°-40°.

後処理

  1. temperatureThe mixture was warmed to 70°
  2. temperatureto maintain
  3. customthe reaction pH at 10.5
  4. temperatureThe mixture was cooled
  5. customwas passed through the mixture at 70°
  6. customInsoluble barium sulfate was removed by filtration
  7. customevaporated to a small volume (30 ml)
  8. additionAddition of methanol (30 ml)
  9. temperatureby cooling

出典と根拠

ORDレコード
ord-50e60c49d739414eafe7377f4fa42f83
出典データセット
uspto-grants-1976_05
特許番号
US03954809

関連ノート

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