Ammonia → HCID 178494684, 화합물

HRID 50378

반응식

HRID 50378 반응식
Cl.COC[C:5]([O:7][CH2:8][CH:9]=[NH:10])=O.[OH:11][CH2:12][C:13]([CH2:15]O)=O.[NH3:17]>C(Cl)Cl>[OH:11][CH2:12][C:13]1[N:17]=[C:9]([CH2:8][O:7][CH3:5])[NH:10][CH:15]=1

참가 물질

5

반응물 3

HCID 222Ammonia2회HCID 670DihydroxyacetoneHCID 57478929Iminoethyl methoxyacetate hydrochloride

생성물 1

HCID 178494684HCID 178494684, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
68 °C

실험 절차

A mixture of 30.6 g (0.20 mol) of iminoethyl methoxyacetate hydrochloride, 18 g (0.20 mol) of 1,3-dihydroxyacetone and 200 mL of liquid ammonia was heated to 68° C. for 3 hours in a stirred autoclave at a pressure of 27 bar (analogously to: P. Dziuron et al., Arch. Pharm. 307, 1974, p.470). Then the ammonia was eliminated and 200 mL of methylene chloride were added. The white precipitate formed was filtered off and washed with methylene chloride. The filtrate was evaporated down and the residue obtained was purified by chromatography (aluminium oxide; methylene chloride/ethanol=90:10 to 85:15). Yield: 26.7 g (94% of theory), C6H10N2O2 (142.20); Rf value: 0.43 (silica gel; methylene chloride/ethanol=9:1); mass spectrum: (M)+=142.

후처리

  1. customThe white precipitate formed
  2. filtrationwas filtered off
  3. washwashed with methylene chloride
  4. customThe filtrate was evaporated down
  5. customthe residue obtained
  6. customwas purified by chromatography (aluminium oxide; methylene chloride/ethanol=90:10 to 85:15)

출처 및 근거

ORD 기록
ord-7e21ca4540c6429c96d42769f9678dad
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06710055B2

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