Hydrochloric Acid → 1-Butyryl-1-(3,4-dichlorophenyl)cyclobutane

HRID 35701ノート

反応式

HRID 35701 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([C:13]#N)[CH2:12][CH2:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8].[CH2:15]([Mg]Br)[CH2:16][CH3:17].C(Br)CC.[Mg].Cl.CC[O:28]CC>O.C1(C)C=CC=CC=1>[C:13]([C:9]1([C:4]2[CH:5]=[CH:6][C:7]([Cl:8])=[C:2]([Cl:1])[CH:3]=2)[CH2:12][CH2:11][CH2:10]1)(=[O:28])[CH2:15][CH2:16][CH3:17]

参加物

9

反応物 6

HCID 313Hydrochloric AcidHCID 3283Diethyl Ether3 回HCID 78401-BromopropaneHCID 5462224MagnesiumHCID 108571341-(3,4-Dichlorophenyl)-1-cyclobutane-carbonitrileHCID 178455851HCID 178455851、化合物

生成物 1

HCID 130833791-Butyryl-1-(3,4-dichlorophenyl)cyclobutane

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1140Toluene溶媒

実験手順

A solution of 1-(3,4-dichlorophenyl)-1-cyclobutanecarbonitrile prepared as described in Example 1 (35.2 g) in ether (100 ml) was added to a solution of propyl magnesium bromide prepared by the reaction of propyl bromide (32 g) with magnesium turnings (6.36 g) in ether (100 ml). The ether was replaced by dry toluene and the mixture heated under reflux for one hour. Water (200 ml) and then concentrated hydrochloric acid (120 ml) were added and the mixture heated under reflux for one hour. The reaction mixture was extracted with ether and after washing and drying the extract yielded a residue from which 1-butyryl-1-(3,4-dichlorophenyl)cyclobutane (b.p. 120°-128° C. at 0.25 mm) was distilled.

後処理

  1. temperaturethe mixture heated
  2. temperatureunder reflux for one hour
  3. temperaturethe mixture heated
  4. temperatureunder reflux for one hour
  5. extractionThe reaction mixture was extracted with ether
  6. washafter washing
  7. customdrying the extract

出典と根拠

ORDレコード
ord-c965ef70e5f54fd2ae4ef4848b72c9f2
出典データセット
uspto-grants-1988_08
特許番号
US04767790

反応ノート

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