Hydrochloric Acid → CID 137208342

HRID 2185595

反応式

HRID 2185595 の反応式
C(OC)(OC)OC.[CH2:8]([C@H:11]([NH2:15])[C:12]([OH:14])=[O:13])[CH2:9][NH2:10].Cl.[C:17](#N)[CH3:18]>CO>[CH3:17][C:18]1[NH:10][CH2:9][CH2:8][C@@H:11]([C:12]([OH:14])=[O:13])[N:15]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6342AcetonitrileHCID 9005Trimethyl orthoformateHCID 134490L-2,4-Diaminobutyric acid

生成物 1

HCID 137208342CID 137208342

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

60 ml of trimethyl orthoformate are dissolved in 400 ml of methanol, and reacted with 30 g of L-diaminobutyric acid×2 HCl at 55° C. with constant stirring. After a reaction time of 2 hours, the solvent is evaporated under reduced pressure, the crude product which remains is dissolved in 50 ml of demineralized water, and the solution is neutralized using NaOH. The compound is subsequently purified on an ion retardation column type BIORAD® AG11A8 (Bio-Rad Laboratories GmbH, Munich, Germany) using demineralized water as the eluent, and the product is dried and recrystallized from methanol. The compound obtained can be identified by means of high-pressure liquid chromatography (HPLC); (for example E. Merck, Darmstadt, Germany, LiChroCART® 125-NH2 5μ, eluent: 80% acetonitrile), and is characterized by the following 13C-NMR data:

後処理

  1. customAfter a reaction time of 2 hours, the solvent is evaporated under reduced pressure
  2. dissolutionthe crude product which remains is dissolved in 50 ml of demineralized water
  3. customThe compound is subsequently purified on an ion retardation column type BIORAD® AG11A8 (Bio-Rad Laboratories GmbH, Munich, Germany)
  4. customthe product is dried
  5. customrecrystallized from methanol
  6. customThe compound obtained can

出典と根拠

ORDレコード
ord-d222339095ca457f9cd2f059345c2353
出典データセット
uspto-grants-2002_06
特許番号
US06403112B2

関連ノート

読み込み中…