Hydrochloric Acid → Ethyl 2-ethylnorleucinate

HRID 1376407

反応式

HRID 1376407 の反応式
C(=[N:8][C:9]([CH2:19][CH3:20])([CH2:15][CH2:16][CH2:17][CH3:18])[C:10]([O:12][CH2:13][CH3:14])=[O:11])C1C=CC=CC=1.Cl>>[CH2:13]([O:12][C:10](=[O:11])[C:9]([NH2:8])([CH2:19][CH3:20])[CH2:15][CH2:16][CH2:17][CH3:18])[CH3:14]

参加物

3

反応物 2

HCID 313Hydrochloric AcidHCID 10107458Ethyl 2-benzylideneamino-2-ethylhexanoate

生成物 1

HCID 42614420Ethyl 2-ethylnorleucinate収率 70%

反応条件

温度
10 °C

実験手順

A solution of the product from step (c) (1 mole) in 1N aqu. HCl (1.2 moles) was stirred for 10 minutes at room temperature, then washed with toluene. The pH of the remaining aqueous phase was adjusted to 7 using 12.5% w/v sodium hydroxide, then cooled to 10° C., further basified to pH 12 and extracted with toluene. The extracts were combined, washed with brine, dried and evaporated in vacuo. The residue was distilled to give the desired product as an oil (70-80% yield).

後処理

  1. washwashed with toluene
  2. extractionextracted with toluene
  3. washwashed with brine
  4. customdried
  5. customevaporated in vacuo
  6. distillationThe residue was distilled

出典と根拠

ORDレコード
ord-39f8b6c166914f39ba69080cb69c09ee
出典データセット
uspto-grants-1997_09
特許番号
US05663165

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