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Hydrochloric Acid → HCID 14650430, 화합물

HRID 1200181
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HRID 1200181 반응식
C1(C([O:9][C:10]2[C:15]([CH3:16])=[CH:14][C:13]([Cl:17])=[CH:12][C:11]=2[C:18](=[O:20])[CH3:19])=O)CCCCC1.[OH-:21].[K+].Cl>N1C=CC=CC=1>[Cl:17][C:13]1[CH:14]=[C:15]([CH3:16])[C:10]([OH:9])=[C:11]([C:18](=[O:20])[CH2:19][C:18]([CH:11]2[CH2:12][CH2:13][CH2:14][CH2:15][CH2:10]2)=[O:21])[CH:12]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 14650427HCID 14650427, 화합물

생성물 1

HCID 14650430HCID 14650430, 화합물수율 154.2%

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
50 °C

실험 절차

2-Acetyl-4-chloro-6-methylphenyl cyclohexanecarboxylate (12 g, 0.0408 mole) was dissolved in pyridine (60 ml) and to the solution was added KOH powder (3 g, 0.0536 mole) with stirring at 50° C. The stirring was continued for 1 hour. The reaction mixture was cooled and poured into diluted hydrochloric acid and extracted with hexane-ethyl acetate (2:1). The extract was washed with water and dried (MgSO4). The solvent was distilled off under reduced pressure. The residue was treated with cold methanol to obtain the title compound (9.27 g) as crystals, yield 77.3%. The crystals were recrystallized from ethyl acetate and hexane to obtained prisms, m.p. 76°-77° C.

후처리

  1. temperatureThe reaction mixture was cooled
  2. extractionextracted with hexane-ethyl acetate (2:1)
  3. washThe extract was washed with water
  4. dry with materialdried (MgSO4)
  5. distillationThe solvent was distilled off under reduced pressure
  6. additionThe residue was treated with cold methanol

출처 및 근거

ORD 기록
ord-8b0e5b82d05a44bcac24a497726f39f1
출처 데이터셋
uspto-grants-1990_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04904690

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