1,3-Dimethyl-2-imidazolidinone → HCID 136403422, 화합물

HRID 258123노트

반응식

HRID 258123 반응식
[N+:1]([N:4]=[C:5]1[NH:10][CH2:9][CH2:8][CH2:7][NH:6]1)([O-:3])=[O:2].[CH:11]([O-:16])([O-])[O:12][CH2:13][CH3:14].CN1[CH2:22][CH2:21]N(C)C1=O>>[CH2:21]([O:16][CH:11]([O:12][CH2:13][CH3:14])[N:6]1[CH2:7][CH2:8][CH2:9][NH:10][C:5]1=[N:4][N+:1]([O-:3])=[O:2])[CH3:22]

참가 물질

4

반응물 3

HCID 66611,3-Dimethyl-2-imidazolidinoneHCID 53630039EthylorthoformateHCID 13624905053360-90-0

생성물 1

HCID 136403422HCID 136403422, 화합물

실험 절차

A mixture of 10 g of 2-nitroiminohexahydropyrimidine, 12.4 g of ethyl orthoformate, 10 ml of 1,3-dimethyl-2-imidazolidinone was heated under reflux for 2.0 hours while removing the resultant distillate by means of the Dean-Stark trap. After cooling to room temperature, the mixture was poured into water, and extracted with ethyl acetate. After washing with water, the extract was dried with anhydrous magnesium sulfate, after which the solvent was distilled off under reduced pressure. The resultant oil was purified by column chromatography [silica gel, eluant: hexane/ethyl acetate (1:2)] to obtain 2.3 g of 1-diethoxymethyl-2-nitroiminohexahydropyrimidine. Typical examples of the compounds of the formula (2) which could be prepared according to the procedures similar to those of Examples 9 to 14 are shown in Table 3.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 2.0 hours
  3. customwhile removing the resultant distillate by means of the Dean-Stark trap
  4. additionthe mixture was poured into water
  5. extractionextracted with ethyl acetate
  6. washAfter washing with water
  7. dry with materialthe extract was dried with anhydrous magnesium sulfate
  8. distillationafter which the solvent was distilled off under reduced pressure
  9. customThe resultant oil was purified by column chromatography [silica gel, eluant: hexane/ethyl acetate (1:2)]

출처 및 근거

ORD 기록
ord-40d94e8037fa46138962a8541ac02788
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05264584

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