Propargyl alcohol → 3-Hydroxy-1-[4-chloro-2-benzoylphenyl]propyne

HRID 2417566ノート

反応式

HRID 2417566 の反応式
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Cl:20][C:21]1[CH:22]=[CH:23][C:24](I)=[C:25]([CH:34]=1)[C:26]([C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)=[O:27].[CH2:36]([OH:39])[C:37]#[CH:38]>[Pd](Cl)Cl.C(NCC)C>[OH:39][CH2:36][C:37]#[C:38][C:24]1[CH:23]=[CH:22][C:21]([Cl:20])=[CH:34][C:25]=1[C:26](=[O:27])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1

参加物

6

反応物 3

HCID 7859Propargyl alcoholHCID 11776TriphenylphosphineHCID 129482625-Chloro-2-iodobenzophenone

生成物 1

HCID 128416443-Hydroxy-1-[4-chloro-2-benzoylphenyl]propyne

試薬・触媒・溶媒 2

HCID 24290Palladium Chloride触媒HCID 8021Diethylamine溶媒

実験手順

A mixture of 0.17 g (1.0 mmole) of palladium chloride, 0.5 g (2.0 mmole) of triphenylphosphine, 0.1 g (0.5 mmole) of cuprous iodide, 15 g (43 mmole) of 5-chloro-2-iodobenzophenone and 60 ml of diethylamine was stirred at room temperature for 20 min. In one portion 6.0 g (107 mmole) of propargyl alcohol was added, and the resulting mixture was stirred for 24 hr. The solvent was removed at reduced pressure and the residue was dissolved in ether. The ether solution was washed with water, dried with anhydrous sodium sulfate, and concentrated at reduced pressure to give the product as a red oil.

後処理

  1. stirringthe resulting mixture was stirred for 24 hr
  2. customThe solvent was removed at reduced pressure
  3. dissolutionthe residue was dissolved in ether
  4. washThe ether solution was washed with water
  5. dry with materialdried with anhydrous sodium sulfate
  6. concentrationconcentrated at reduced pressure

出典と根拠

ORDレコード
ord-0a318b4333564776ac286fe3165a3d3f
出典データセット
uspto-grants-1984_09
特許番号
US04469633

反応ノート

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