Ammonia → HCID 178494684、化合物

HRID 50378

反応式

HRID 50378 の反応式
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

参加物

5

反応物 3

HCID 222Ammonia2 回HCID 670DihydroxyacetoneHCID 57478929Iminoethyl methoxyacetate hydrochloride

生成物 1

HCID 178494684HCID 178494684、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
68 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-7e21ca4540c6429c96d42769f9678dad
出典データセット
uspto-grants-2004_03
特許番号
US06710055B2

関連ノート

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