Hydrochloric Acid → Hydrochloric Acid

HRID 2166014ノート

反応式

HRID 2166014 の反応式
[CH3:1][CH:2]([CH2:4][C:5](=O)[CH2:6][CH:7]([CH3:9])[CH3:8])[CH3:3].C([O-])(=O)C.[NH4+].C([BH3-])#[N:17].[Na+].[ClH:20]>CO>[ClH:20].[CH3:1][CH:2]([CH2:4][CH:5]([NH2:17])[CH2:6][CH:7]([CH3:9])[CH3:8])[CH3:3].[ClH:20]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 7958Isobutyl ketoneHCID 517165Ammonium AcetateHCID 5003444Sodium cyanoborohydride

生成物 2

HCID 313Hydrochloric AcidHCID 230417822,6-dimethylheptan-4-amine hydrochloride

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 2,6 -dimethyl-4 -heptanone (2.84 g, 20 mmol), ammonium acetate (15.4 g, 200 mmol) and sodium cyanoborohydride (0.93 g, 14 mmol) in methanol (75 mL) was stirred at room temperature for 20 hours. After cooling in an ice bath, the reaction mixture was acidified with concentrated HCl and concentrated under reduced pressure at 35° . The residue was partitioned between ethyl ether and water and the aqueous portion removed and made basic with 40% NaOH solution. Product was extracted into ethyl ether which was then washed with brine, dried (Na2SO4), filtered and concentrated to 1.22 g of product. Conversion to the HCl salt and recrystallation from MeOH-EtOAc gave 1.04 of pure HCl salt, mp 248°-50° dec.

後処理

  1. temperatureAfter cooling in an ice bath
  2. concentrationconcentrated under reduced pressure at 35°
  3. customThe residue was partitioned between ethyl ether and water
  4. customthe aqueous portion removed
  5. extractionProduct was extracted into ethyl ether which
  6. washwas then washed with brine
  7. dry with materialdried (Na2SO4)
  8. filtrationfiltered
  9. concentrationconcentrated to 1.22 g of product

出典と根拠

ORDレコード
ord-fba9b53cc90b4c928ef425f2a9b3d144
出典データセット
uspto-grants-1990_07
特許番号
US04943561

反応ノート

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