Oxirane, [[4-[2-(2-methylpropoxy)ethoxy]phenoxy]methyl]- → HCID 20222108, 화합물

HRID 980166노트

반응식

HRID 980166 반응식
[CH3:1][CH:2]([CH3:19])[CH2:3][O:4][CH2:5][CH2:6][O:7][C:8]1[CH:18]=[CH:17][C:11]([O:12][CH2:13][CH:14]2[O:16][CH2:15]2)=[CH:10][CH:9]=1.[NH2:20][CH2:21][CH2:22][NH:23][C:24]([N:26]([CH3:28])[CH3:27])=[O:25]>C(O)(C)C>[CH3:27][N:26]([CH3:28])[C:24]([NH:23][CH2:22][CH2:21][NH:20][CH2:15][CH:14]([OH:16])[CH2:13][O:12][C:11]1[CH:17]=[CH:18][C:8]([O:7][CH2:6][CH2:5][O:4][CH2:3][CH:2]([CH3:19])[CH3:1])=[CH:9][CH:10]=1)=[O:25]

참가 물질

4

반응물 2

HCID 10635469Oxirane, [[4-[2-(2-methylpropoxy)ethoxy]phenoxy]methyl]-HCID 20383014N'-(2-Aminoethyl)-N,N-dimethylurea

생성물 1

HCID 20222108HCID 20222108, 화합물

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

8 g of 3-(4-(2-(2-methylpropoxy)ethoxy)phenoxy)-1,2-epoxypropane and 14 g of N-2-aminoethyl-N',N'-dimethylurea was warmed (60°-70° C.) in 150 ml of isopropanol over night. The mixture was evaporated and the residue dissolved in ethyl acetate. The ethyl acetate phase was washed with water (twice), fresh water was then added and pH lowered to 5 with hydrochloric acid. Fresh ethyl acetate was then added to the water phase and pH was rised to 9.5. The organic phase was separated off, dried, and evaporated. The residue was recrystallized from a small amount of ethyl acetate. Yield 3 g. M.p. 75° C. (base). The structure was determined using NMR-analysis.

후처리

  1. customThe mixture was evaporated
  2. dissolutionthe residue dissolved in ethyl acetate
  3. washThe ethyl acetate phase was washed with water (twice), fresh water
  4. additionwas then added
  5. additionFresh ethyl acetate was then added to the water phase and pH
  6. customThe organic phase was separated off
  7. customdried
  8. customevaporated
  9. customThe residue was recrystallized from a small amount of ethyl acetate

출처 및 근거

ORD 기록
ord-54c1b940729641c49eefa387cfa091b9
출처 데이터셋
uspto-grants-1987_01
특허 번호
US04636501

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