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

HRID 980166ノート

反応式

HRID 980166 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 20222108HCID 20222108、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-54c1b940729641c49eefa387cfa091b9
出典データセット
uspto-grants-1987_01
特許番号
US04636501

反応ノート

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