Methanol → HCID 21485772、化合物

HRID 1077141

反応式

HRID 1077141 の反応式
[C:1]([O:4][C:5]1[CH:6]=[C:7]([CH2:11][CH2:12][CH2:13][C:14](=[O:22])[CH2:15][CH2:16]N(CC)CC)[CH:8]=[CH:9][CH:10]=1)(=[O:3])[CH3:2].C(OC1C=C(CCCC(=O)C=C)C=CC=1)(=O)C.[CH3:40][CH:41]1[C:45](=[O:46])[CH2:44][CH2:43][C:42]1=[O:47].CO>[OH-].[K+].C(Cl)(Cl)Cl>[C:1]([O:4][C:5]1[CH:6]=[C:7]([CH2:11][CH2:12][CH2:13][C:14](=[O:22])[CH2:15][CH2:16][C:41]2([CH3:40])[C:45](=[O:46])[CH2:44][CH2:43][C:42]2=[O:47])[CH:8]=[CH:9][CH:10]=1)(=[O:3])[CH3:2]

参加物

7

反応物 4

HCID 887MethanolHCID 130052-Methyl-1,3-cyclopentanedioneHCID 214854206-m-Acetoxyphenyl-1-diethylaminohexan-3-oneHCID 214855806-m-Acetoxyphenylhex-1-en-3-one

生成物 1

HCID 21485772HCID 21485772、化合物

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 14797Potassium Hydroxide溶媒

実験手順

Reflux a mixture of 6-(m-acetoxyphenyl)-1-diethylaminohexan-3-one and 6-(m-acetoxyphenyl)hex-1-en-3-one (1 g), with 2-methylcyclopentane-1,3-dione (1.5 g) in 0.12% methanolic potassium hydroxide (6 cc) for 18 hours. Remove methanol (2 cc) under reduced pressure and add chloroform (60 cc). Wash the solution in turn with dilute sulfuric acid (25 cc), saturated potassium bicarbonate solution, and brine; dry and evaporate the solvent. The product (0.8 g) is the adduct 2-(6-m-acetoxyphenyl-3-oxohexyl)-2-methylcyclopentane-1,3-dione in admixture with some of the corresponding free phenol; infrared absorption: 2.86 to 3.08 (broad low-intensity band), 5.71, 5.81, 5.85, and 8.26 μ.

後処理

  1. temperatureReflux
  2. washWash the solution in turn with dilute sulfuric acid (25 cc), saturated potassium bicarbonate solution, and brine
  3. customdry
  4. customevaporate the solvent
  5. customabsorption

出典と根拠

ORDレコード
ord-8782780bea62495b8605cb452e75635c
出典データセット
uspto-grants-1976_05
特許番号
US03959322

関連ノート

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