Ammonia → 6-chlorohexyl(2E)-3-(4-hydroxyphenyl)prop-2-enoate

HRID 523329노트

반응식

HRID 523329 반응식
N.C(OC([O:7][C:8]1[CH:13]=[CH:12][C:11](/[CH:14]=[CH:15]/[C:16]([O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][Cl:25])=[O:17])=[CH:10][CH:9]=1)=O)C>CC(C)=O.N1C=CC=CC=1>[OH:7][C:8]1[CH:9]=[CH:10][C:11](/[CH:14]=[CH:15]/[C:16]([O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][Cl:25])=[O:17])=[CH:12][CH:13]=1

참가 물질

5

반응물 2

HCID 222AmmoniaHCID 867326476-chlorohexyl(2E)-3-{4-[(ethoxycarbonyl)oxy]phenyl}prop-2-enoate

생성물 1

HCID 867326486-chlorohexyl(2E)-3-(4-hydroxyphenyl)prop-2-enoate수율 100.2%

시약·촉매·용매 2

HCID 180Acetone용매HCID 1049Pyridine용매

실험 절차

A 25% NH3 solution diluted in 780 mL of acetone is added dropwise to a solution of 89.3 g (247 mmol) of 6-chlorohexyl(2E)-3-{4-[(ethoxycarbonyl)oxy]phenyl}prop-2-enoate in 752 mL of pyridine. The mixture is allowed to stir for 20 hours at room temperature. The reaction mixture is then partitioned between ethylacetate and water. The organic phase is then washed repeatedly with water, dried over sodium sulfate, filtered off and concentrated by rotary evaporation. The solid is dried under vacuum to yield 70 g (100%) of pure 6-chlorohexyl(2E)-3-(4-hydroxyphenyl)prop-2-enoate as a white powder.

후처리

  1. customThe reaction mixture is then partitioned between ethylacetate and water
  2. washThe organic phase is then washed repeatedly with water
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered off
  5. concentrationconcentrated by rotary evaporation
  6. customThe solid is dried under vacuum

출처 및 근거

ORD 기록
ord-1448c00ac21541c1a4a3da575b37b787
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09334366B2

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