Diethyl Ether → HCID 86740393, 화합물

HRID 465053노트

반응식

HRID 465053 반응식
[CH2:1]([O:3][C:4](=[O:8])[CH2:5][NH:6][CH3:7])[CH3:2].[CH2:9](N(CC)CC)C.[Cl:16][C:17](Cl)(CCl)[C:18]#[N:19].C(OCC)C>O1CCCC1>[Cl:16][C:17](=[CH:7][N:6]([CH2:5][C:4]([O:3][CH2:1][CH3:2])=[O:8])[CH3:9])[C:18]#[N:19]

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 8471TriethylamineHCID 131332,2,3-TrichloropropanenitrileHCID 95849Glycine, N-methyl-, ethyl ester

생성물 1

HCID 86740393HCID 86740393, 화합물수율 96%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A mixture of sarcosine ethyl ester (58.5 g, 0.499 mol), tetrahydrofuran (200 ml) and triethylamine (101.2 g, 1 mol) is added dropwise within 15 minutes to a solution of 2,2,3-trichloropropionitrile (79.0, 0.499 mol) in tetrahydrofuran (200 ml). Within 1 hour, the temperature of the mixture rises spontaneously to 30° C. To complete the reaction, the mixture is then refluxed for 3 hours. It is left to cool, stirred into diethyl ether (4 liters), filtered to remove the precipitated triethylamine hydrochloride and the etheral solution is concentrated. The residue is distilled under high vacuum to give a colorless oil (97.1 g), boiling point 0.3 mm Hg 120°-130° C. containing both isomers in a ratio of approximetely 1:1 according to 1H-NMR spectroscopy. An isomer, presumably the isomer of (E) configuration, crystallises out of this oil occasionally, mp. 57° C.

후처리

  1. customrises spontaneously to 30° C
  2. customthe reaction
  3. temperaturethe mixture is then refluxed for 3 hours
  4. waitIt is left
  5. temperatureto cool
  6. filtrationfiltered
  7. customto remove the precipitated triethylamine hydrochloride
  8. concentrationthe etheral solution is concentrated
  9. distillationThe residue is distilled under high vacuum

출처 및 근거

ORD 기록
ord-b02f2fea7a794aba9f67be2f82feb21e
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04550107

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