Hydrochloric Acid → (S)-2-CHLORO-4-METHYL-N-VALERIC ACID

HRID 1088194ノート

反応式

HRID 1088194 の反応式
N[C@H:2]([C:7]([OH:9])=[O:8])[CH2:3][CH:4]([CH3:6])[CH3:5].[ClH:10].NC(N)=O>[N+]([O-])(O)=O>[Cl:10][C@@H:2]([CH2:3][CH:4]([CH3:6])[CH3:5])[C:7]([OH:9])=[O:8]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 1176UreaHCID 6106L-Leucine

生成物 1

HCID 12732683(S)-2-CHLORO-4-METHYL-N-VALERIC ACID

試薬・触媒・溶媒 1

HCID 944Nitric Acid溶媒

反応条件

温度
80 °C

実験手順

L-(+)-Leucine (10 g, 0.076 moles) is mixed with 24 mL of concentrated HCl and 10 mL of concentrated HNO3 with the addition of 2 g of urea and subsequently heated for 1 hour at 80° C. and then for 1 hour at 50° C. on a water bath (complete dissolution of the acid with heavy foaming). After cooling, the solution is extracted with ether several times, the ether extract is washed with water and dried over calcium chloride, the solvent is distilled off in a rotary evaporator and the residue is fractionally distilled under vacuum.

後処理

  1. dissolutionfor 1 hour at 50° C. on a water bath (complete dissolution of the acid with heavy foaming)
  2. temperatureAfter cooling
  3. extractionthe solution is extracted with ether several times
  4. extractionthe ether extract
  5. washis washed with water
  6. dry with materialdried over calcium chloride
  7. distillationthe solvent is distilled off in a rotary evaporator
  8. distillationthe residue is fractionally distilled under vacuum

出典と根拠

ORDレコード
ord-2c00c676e0c1468a958b90074c5ddc6b
出典データセット
uspto-grants-1990_10
特許番号
US04961876

反応ノート

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