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Hydrochloric Acid → HCID 14650430、化合物

HRID 1200181
ノート
印刷プレビュー

反応式

HRID 1200181 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 14650427HCID 14650427、化合物

生成物 1

HCID 14650430HCID 14650430、化合物収率 154.2%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
50 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8b0e5b82d05a44bcac24a497726f39f1
出典データセット
uspto-grants-1990_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04904690

反応ノート

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