Hydrochloric Acid → Decanoic acid, 2-methyl-

HRID 846548

反応式

HRID 846548 の反応式
S(=O)(=O)(O)O.[CH3:6][CH:7]([CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[CH2:8][OH:9].[Mn]([O-])(=O)(=O)=[O:19].[K+].S([O-])(O)=O.[Na+].Cl>O>[CH3:6][CH:7]([CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[C:8]([OH:19])=[O:9]

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 1118Sulfuric AcidHCID 867761-Decanol, 2-methyl-HCID 516875Potassium PermanganateHCID 23665763Sodium Bisulfite

生成物 1

HCID 91167Decanoic acid, 2-methyl-収率 268.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

After 14.6 g of concentrated sulfuric acid and 8.6 g (50 mmol) of (-)-2-methyldecanol were added to 96 ml of water, 16.4 g (10.4 mmol) of potassium permanganate was added dropwise over 4 hours while the reaction temperature was held below 25° C. The thus obtained reaction mixture was poured into 300 ml of ice water, added with 30 g of sodium hydrogen sulfite, adjusted to pH of not more than 1 with hydrochloric acid, extracted with ether and then extracted with a 10% aqueous solution of sodium hydroxide. This extract was added with hydrochloric acid to adjust pH to not more than 1 and again extracted with chloroform. The thus obtained extract was washed with water, dried, concentrated, and distilled under a reduced pressure (0.4 mmHg, 116°~120° C.) to obtain 5.2 g (yield 63%) of (+)-2-metyl decanoic acid.

後処理

  1. additionwas added dropwise over 4 hours while the reaction temperature
  2. customwas held below 25° C
  3. customThe thus obtained reaction mixture
  4. extractionextracted with ether
  5. extractionextracted with a 10% aqueous solution of sodium hydroxide
  6. additionThis extract was added with hydrochloric acid
  7. extractionagain extracted with chloroform
  8. customThe thus obtained
  9. extractionextract
  10. washwas washed with water
  11. customdried
  12. concentrationconcentrated
  13. distillationdistilled under a reduced pressure (0.4 mmHg, 116°~120° C.)

出典と根拠

ORDレコード
ord-1bc121b5fb044321bf7fdcd54a841e11
出典データセット
uspto-grants-1992_08
特許番号
US05137653

関連ノート

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