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Hydrochloric Acid → 3-[4-(6-Acetoxy-2,5,7,8-tetramethylchroman-2-ylmethoxy)phenyl]-2-chloropropionic acid

HRID 1589700
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HRID 1589700 반응식
[C:1]([O:4][C:5]1[C:6]([CH3:34])=[C:7]2[C:12](=[C:13]([CH3:16])[C:14]=1[CH3:15])[O:11][C:10]([CH2:18][O:19][C:20]1[CH:25]=[CH:24][C:23]([CH2:26][CH:27]([Cl:33])[C:28]([O:30]CC)=[O:29])=[CH:22][CH:21]=1)([CH3:17])[CH2:9][CH2:8]2)(=[O:3])[CH3:2].[OH-].[Na+].Cl>C(O)C.O1CCCC1>[C:1]([O:4][C:5]1[C:6]([CH3:34])=[C:7]2[C:12](=[C:13]([CH3:16])[C:14]=1[CH3:15])[O:11][C:10]([CH2:18][O:19][C:20]1[CH:21]=[CH:22][C:23]([CH2:26][CH:27]([Cl:33])[C:28]([OH:30])=[O:29])=[CH:24][CH:25]=1)([CH3:17])[CH2:9][CH2:8]2)(=[O:3])[CH3:2]
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참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 13605832HCID 13605832, 화합물

생성물 1

HCID 134888703-[4-(6-Acetoxy-2,5,7,8-tetramethylchroman-2-ylmethoxy)phenyl]-2-chloropropionic acid

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran
용매

실험 절차

0.16 g of ethyl 3-[4-(6-acetoxy-2,5,7,8-tetramethylchroman-2-ylmethoxy)phenyl]-2-chloropropionate was dissolved in a mixture of 1.5 ml of 99.5% ethanol and 0.2 ml of tetrahydrofuran. 265 mg of a 9.55% w/w aqueous solution of sodium hydroxide were added dropwise, under a nitrogen stream at 0°-4° C., to the resulting mixture. The mixture was then reacted for a further 20 hours at 0°-5° C., after which it was neutralized, whilst ice-cooling, by adding 0.68 g of a 10% w/w aqueous solution of hydrochloric acid. The solvent was then distilled off under reduced pressure. The separated light reddish oil was further extracted with chloroform, and the chloroform extract was washed with water and dried over anhydrous sodium sulfate. The crude product obtained by distilling off the chloroform under reduced pressure was subjected to column chromatography through silica gel and the desired 3-[4-(6-acetoxy-2,5,7,8-tetramethylchroman-2-ylmethoxy)phenyl]-2-chloropropionic acid was obtained from the fractions eluted with a 20:1 by volume mixture of benzene and 99.5% ethanol. Rf value on thin layer chromatography: 0.6 (tailing) [silica gel; developing solvent; benzene:99.5% ethanol=4:1 by volume].

후처리

  1. customThe mixture was then reacted for a further 20 hours at 0°-5° C.
  2. temperaturecooling
  3. distillationThe solvent was then distilled off under reduced pressure
  4. extractionThe separated light reddish oil was further extracted with chloroform
  5. extractionthe chloroform extract
  6. washwas washed with water
  7. dry with materialdried over anhydrous sodium sulfate
  8. customThe crude product obtained
  9. distillationby distilling off the chloroform under reduced pressure

출처 및 근거

ORD 기록
ord-53a40f96d925483782c2b368d8433414
출처 데이터셋
uspto-grants-1986_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04572912

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