Ethanolamine → 1,2-Diphenyl-2-methoxy-1-(2-hydroxyethylimino)ethane

HRID 1381516

반응식

HRID 1381516 반응식
[CH2:1]([CH2:3][NH2:4])[OH:2].[CH3:5][O:6][CH:7]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[C:8]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)=O.O>CO>[C:10]1([C:8](=[N:4][CH2:3][CH2:1][OH:2])[CH:7]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[O:6][CH3:5])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

참가 물질

5

반응물 3

HCID 700EthanolamineHCID 962WaterHCID 98097Methyl Benzoin2회

생성물 1

HCID 212761221,2-Diphenyl-2-methoxy-1-(2-hydroxyethylimino)ethane수율 94%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
120 °C

실험 절차

Ethanolamine, 8.34 g (0.137 mole) and 4.52 g (0.020 mole) of 2-methoxy-1,2-diphenylethanone were mixed together and heated at 120° C. under a gentle stream of nitrogen for 2 hr. Mass spec analysis indicated none of the 2-methoxy-1,2-diphenylethanone remained. The mixture stood at ambient temperature for 16 hr, after which it was dissolved in 20 ml of methanol. The solution was poured into 100 ml of water. A yellow oil separated which became semisolid after 1 hr. The semisolid was extracted twice with 50 ml portions of methylene chloride. The extract was dried over magnesium sulfate, filtered, and concentrated to give 5.04 g of yellow oil (94%) which began to solidify on standing. Trituration with petroleum ether gave 2.19 g of off-white solid after filtration. The filtrate was concentrated to give an additional 2.25 g of yellow oil which was identical to the white solid and which crystallized on standing.

후처리

  1. customA yellow oil separated which
  2. customafter 1 hr
  3. extractionThe semisolid was extracted twice with 50 ml portions of methylene chloride
  4. dry with materialThe extract was dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-45156a2307b44110be543f41b117cfc9
출처 데이터셋
uspto-grants-1989_02
특허 번호
US04803200

연결된 노트

불러오는 중…