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Potassium Iodide → 2-Imidazolidinone, 1-((4-chlorophenyl)methyl)-

HRID 1658818
ノート
印刷プレビュー

反応式

HRID 1658818 の反応式
[NH:1]1[CH2:5][CH2:4][NH:3][C:2]1=[O:6].C(=O)([O-])[O-].[K+].[K+].[I-].[K+].[Cl:15][C:16]1[CH:23]=[CH:22][C:19]([CH2:20]Cl)=[CH:18][CH:17]=1>CS(C)=O.O>[Cl:15][C:16]1[CH:23]=[CH:22][C:19]([CH2:20][N:1]2[CH2:5][CH2:4][NH:3][C:2]2=[O:6])=[CH:18][CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 4875Potassium IodideHCID 77231-Chloro-4-(chloromethyl)benzeneHCID 84532-ImidazolidinoneHCID 11430Potassium Carbonate

生成物 1

HCID 50764812-Imidazolidinone, 1-((4-chlorophenyl)methyl)-収率 92%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide
溶媒
HCID 962Water溶媒

実験手順

A 21.5 g (0.25 mole) portion of 2-imidazolidinone in 300 ml of dimethylsulfoxide was treated with 34.5 g (0.25 mole) of potassium carbonate, 10 g (0.06 mole) of potassium iodide and 40.5 g (0.25 mole) of 4-chlorobenzyl chloride. The reaction mixture was heated to 100° over 0.3 hours, held at 100° with rapid stirring for 1.3 hours and poured into 1.3 l of water. The aqueous mixture was extracted with 1.3 l of chloroform. The chloroform extract was washed with 150 ml of water, dried over magnesium sulfate for 3 hours and filtered. The filtrate was concentrated to dryness to give 49 g (92%) a light yellow oil which crystallized.

後処理

  1. temperatureThe reaction mixture was heated to 100° over 0.3 hours
  2. customheld at 100°
  3. extractionThe aqueous mixture was extracted with 1.3 l of chloroform
  4. extractionThe chloroform extract
  5. washwas washed with 150 ml of water
  6. dry with materialdried over magnesium sulfate for 3 hours
  7. filtrationfiltered
  8. concentrationThe filtrate was concentrated to dryness

出典と根拠

ORDレコード
ord-6b90fcd9ea3c4192b711a5f5685fe479
出典データセット
uspto-grants-1976_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03966758

反応ノート

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