Hydrochloric Acid → CID 137208342

HRID 1107218

반응식

HRID 1107218 반응식
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

참가 물질

6

반응물 4

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

생성물 1

HCID 137208342CID 137208342

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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: 176.8, 161.2, 53.8, 37.9, 22.0, 18.7 ppm (relative to TMS); (Galinski E. A., Pfeiffer H. P., Truper H. G. (1985) Eur. J. Biochem. 149, 135-139).

후처리

  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

출처 및 근거

ORD 기록
ord-baef40fea698453b9508ff2d92d91117
출처 데이터셋
uspto-grants-2000_05
특허 번호
US06060071

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