Sulfuric Acid → Canthaxanthin

HRID 2057737

反応式

HRID 2057737 の反応式
Cl([O-])(=O)=O.[Na+].[I-].[Na+].[CH3:8][C:9]1[CH:14]([OH:15])[CH2:13][CH2:12][C:11]([CH3:17])([CH3:16])[C:10]=1/[CH:18]=[CH:19]/[C:20](/[CH3:49])=[CH:21]/[CH:22]=[CH:23]/[C:24](/[CH3:48])=[CH:25]/[CH:26]=[CH:27]/[CH:28]=[C:29](\[CH3:47])/[CH:30]=[CH:31]/[CH:32]=[C:33](\[CH3:46])/[CH:34]=[CH:35]/[C:36]1[C:41]([CH3:43])([CH3:42])[CH2:40][CH2:39][CH:38]([OH:44])[C:37]=1[CH3:45].S(=O)(=O)(O)O.C(=O)([O-])[O-].[Na+].[Na+]>O.C(Cl)(Cl)Cl>[CH3:45][C:37]1[C:38](=[O:44])[CH2:39][CH2:40][C:41]([CH3:42])([CH3:43])[C:36]=1/[CH:35]=[CH:34]/[C:33](/[CH3:46])=[CH:32]/[CH:31]=[CH:30]/[C:29](/[CH3:47])=[CH:28]/[CH:27]=[CH:26]/[CH:25]=[C:24](\[CH3:48])/[CH:23]=[CH:22]/[CH:21]=[C:20](\[CH3:49])/[CH:19]=[CH:18]/[C:10]1[C:11]([CH3:17])([CH3:16])[CH2:12][CH2:13][C:14](=[O:15])[C:9]=1[CH3:8]

参加物

8

反応物 5

HCID 1118Sulfuric AcidHCID 5238Sodium IodideHCID 10340Sodium CarbonateHCID 516902Sodium ChlorateHCID 11757703β,β-Carotene-4,4'-diol

生成物 1

HCID 5281227Canthaxanthin収率 94,872.398%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6212Chloroform溶媒

実験手順

An aqueous solution of 3.2 g of sodium chlorate and 20 mg of sodium iodide, dissolved in 20 ml of water, is added to 500 mg of racemic isozeaxanthin dissolved in 50 ml of chloroform, the two-phase mixture is stirred thoroughly at room temperature, and 5 ml of 0.01N sulfuric acid is added. After an hour, the mixture is neutralized with dilute sodium carbonate solution, the phases are separated, and the organic phase is washed with water and dried over sodium sulfate. The solvent is distilled off under reduced pressure, 50 ml of heptane is added to the residue, and the whole is refluxed for 1 hour. After cooling, filtration gives 471 g (94% of theory) of canthaxanthin.

後処理

  1. waitAfter an hour
  2. customthe phases are separated
  3. washthe organic phase is washed with water
  4. dry with materialdried over sodium sulfate
  5. distillationThe solvent is distilled off under reduced pressure, 50 ml of heptane
  6. additionis added to the residue
  7. temperaturethe whole is refluxed for 1 hour
  8. temperatureAfter cooling
  9. filtrationfiltration

出典と根拠

ORDレコード
ord-d995584d61d8457c8560b1023dcc81b7
出典データセット
uspto-grants-1980_07
特許番号
US04212827

関連ノート

読み込み中…