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Potassium thiocyanate → 1-(4,6-Difluoroindan-1-yl)-1,3-dihydroimidazole-2-thione

HRID 1735880
ノート
印刷プレビュー

反応式

HRID 1735880 の反応式
[F:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[C:7]2[C:3]=1[CH2:4][CH2:5][CH:6]2[NH:12][CH2:13][CH:14](OC)OC.[S-:19][C:20]#[N:21].[K+]>Cl.C(O)C.O>[F:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[C:7]2[C:3]=1[CH2:4][CH2:5][CH:6]2[N:12]1[CH:13]=[CH:14][NH:21][C:20]1=[S:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 516872Potassium thiocyanateHCID 19699493(4,6-Difluoroindan-1-yl)-(2,2-dimethoxyethyl)amine

生成物 1

HCID 196992771-(4,6-Difluoroindan-1-yl)-1,3-dihydroimidazole-2-thione収率 48.4%

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid溶媒HCID 702Ethanol溶媒HCID 962
Water
溶媒
2 回

実験手順

A mixture of (4,6-difluoroindan-1-yl)-(2,2-dimethoxyethyl)amine (11.68 g, 45.9 mmol), potassium thiocyanate (4.46 g, 45.9 mmol) in 21.6 mL of 12N hydrochloric acid, 86 mL of ethanol and 86 mL of water was heated at 80° to 85° C. for 15 hours. The mixture was cooled in an ice bath and diluted with water giving a crystalline material. The material was isolated by filtration and the filter residue was rinsed with cold ethanol (2×25 mL) and 50 mL of diethyl ether. Drying gave 1-(4,6-difluoroindan-1-yl)-1,3-dihydroimidazole-2-thione (5.65 g, 22.2 mmol), m.p. 205°-207° C.

後処理

  1. temperaturewas heated at 80° to 85° C. for 15 hours
  2. temperatureThe mixture was cooled in an ice bath
  3. customThe material was isolated by filtration
  4. washthe filter residue was rinsed with cold ethanol (2×25 mL) and 50 mL of diethyl ether
  5. customDrying

出典と根拠

ORDレコード
ord-83357fe41934412d8b2d30b3d4838146
出典データセット
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05538988

反応ノート

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