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18-Crown-6 → 1-(4-[4-Chloro-1-naphthoxy]-3,5-dichlorophenyl)-3-(2,6-difluorobenzoyl)thiourea

HRID 978475
ノート
印刷プレビュー

反応式

HRID 978475 の反応式
[S-:1][C:2]#[N:3].[K+].C1OCCOCCOCCOCCOCCOC1.[F:23][C:24]1[CH:32]=[CH:31][CH:30]=[C:29]([F:33])[C:25]=1[C:26](Cl)=[O:27].[Cl:34][C:35]1[C:44]2[C:39](=[CH:40][CH:41]=[CH:42][CH:43]=2)[C:38]([O:45][C:46]2[C:52]([Cl:53])=[CH:51][C:49]([NH2:50])=[CH:48][C:47]=2[Cl:54])=[CH:37][CH:36]=1>CC#N.O>[Cl:34][C:35]1[C:44]2[C:39](=[CH:40][CH:41]=[CH:42][CH:43]=2)[C:38]([O:45][C:46]2[C:47]([Cl:54])=[CH:48][C:49]([NH:50][C:2]([NH:3][C:26](=[O:27])[C:25]3[C:24]([F:23])=[CH:32][CH:31]=[CH:30][C:29]=3[F:33])=[S:1])=[CH:51][C:52]=2[Cl:53])=[CH:37][CH:36]=1
参加物反応条件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 2855718-Crown-6HCID 874382,6-Difluorobenzoyl chlorideHCID 516872Potassium thiocyanateHCID 138271123,5-Dichloro-4-[(4-chloronaphthalen-1-yl)oxy]aniline

生成物 1

HCID 138271131-(4-[4-Chloro-1-naphthoxy]-3,5-dichlorophenyl)-3-(2,6-difluorobenzoyl)thiourea

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6342Acetonitrile溶媒2 回

反応条件

温度
0 °C

実験手順

To a mixture of 1.4 g of potassium thiocyanate and 1.0 mg of 18-Crown-6 in 15 ml CH3CN which was cooled to 0° C. and placed under an atmosphere of nitrogen was slowly added a solution of 23 g of 2,6-diflurobenzoyl chloride in 15 ml of CH3CN. The reaction mixture was stirred for 0.5 hr at 0° C. and then allowed to warm to room temperature. After 0.5 hr at an IR spectrum of an aliquot indicated complete disappearance of the acid chloride. To the reaction mixture was then added 4.0 g of 4-(4-chloro-1-naphthoxy)-3,5-dichloroaniline as a powder. After 0.5 hr at ambient temperature the reaction mixture was poured into 125 ml of cold water. A buff colored solid precipitated and was filtered. The filter cake was then washed with 120 ml of a 5:1 H2O:CH3CN solution. The crystals were then dried overnight in a vacuum oven at 50° C. This afforded 5.6 g of the desired thiourea as a pale yellow crystalline powder. mp 193°-195° C. NMR (D6 -DMSO): 6.43 (d, J-10 Hz, 1H), 7.0-817 (m, 10H contains singlet at 8.13), 12.35 (s, 1H), 12.62 (s, 1H).

後処理

  1. temperatureto warm to room temperature
  2. waitAfter 0.5 hr at an IR spectrum of an aliquot indicated complete
  3. customprecipitated
  4. filtrationwas filtered
  5. washThe filter cake was then washed with 120 ml of a 5:1 H2O
  6. customThe crystals were then dried overnight in a vacuum oven at 50° C

出典と根拠

ORDレコード
ord-4fa8ef48f1144f928523ac509f49b51e
出典データセット
uspto-grants-1987_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04665097

反応ノート

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