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Hydrochloric Acid → HCID 88658672, 화합물

HRID 652453
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HRID 652453 반응식
Cl[C:2]1[CH:7]=[C:6]([C:8]#[N:9])[CH:5]=[CH:4][C:3]=1O.[CH2:11]([CH:13]1O[CH2:14]1)[Cl:12].[OH-:16].[K+].Cl>C(O)C.O>[Cl:12][CH2:11][CH2:13][CH2:14][C:3]1[CH:4]=[CH:5][C:6]([C:8]#[N:9])=[C:7]2[O:16][C:2]=12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 7835EpichlorohydrinHCID 14797Potassium HydroxideHCID 2735739Benzonitrile, 3-chloro-4-hydroxy-

생성물 1

HCID 88658672HCID 88658672, 화합물수율 42.8%

시약·촉매·용매 2

HCID 702Ethanol용매2회
HCID 962
Water
용매

실험 절차

While a solution of 2-chloro-4-cyanophenol (50 g) and epichlorohydrin (60.3 g) in ethanol (55 ml) was refluxed, a solution of potassium hydroxide (21.9 g) in ethanol (90 ml) was added dropwise over a period of 40 minutes and the reaction mixture was further refluxed for 100 minutes. After the mixture was cooled, water (50 ml) was added thereto and it was neutralized with 1N hydrochloric acid. After the solvent was distilled off, the residue was extracted with diethyl ether. The extract was dried (over magnesium sulfate) and the diethyl ether was distilled off. The residue was distilled under reduced pressure to give 27 g of 3-chloro-4-(2,3-epoxy)propylbenzonitrile as a colorless oil. After crystallization, the crystals are recrystallized from isopropyl ether-ethyl acetate to give colorless needles. m.p. 71.0°-71.8° C.

후처리

  1. temperaturethe reaction mixture was further refluxed for 100 minutes
  2. temperatureAfter the mixture was cooled
  3. distillationAfter the solvent was distilled off
  4. extractionthe residue was extracted with diethyl ether
  5. dry with materialThe extract was dried (over magnesium sulfate)
  6. distillationthe diethyl ether was distilled off
  7. distillationThe residue was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-b2f8bba8dc834e3a82199112b1c1bfd9
출처 데이터셋
uspto-grants-1987_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04672073

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