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

HRID 863069
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인쇄 미리보기

반응식

HRID 863069 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

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

생성물 1

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

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매HCID 702Ethanol용매HCID 962
Water
용매
2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-469010e7433e499a8cf7b1a9783f48f8
출처 데이터셋
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05719280

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