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Sodium Methoxide → HCID 15008938、化合物

HRID 654268
ノート
印刷プレビュー

反応式

HRID 654268 の反応式
[CH3:1][O-:2].[Na+].[CH3:4][NH:5][C:6]1[N:11]=[C:10](C(Cl)(Cl)Cl)[N:9]=[C:8]([C:16]([F:19])([F:18])[F:17])[N:7]=1>CO.O.Cl>[CH3:1][O:2][C:10]1[N:11]=[C:6]([NH:5][CH3:4])[N:7]=[C:8]([C:16]([F:19])([F:18])[F:17])[N:9]=1
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 10942334Sodium Methoxide2 回HCID 15008937N-Methyl-4-(trichloromethyl)-6-(trifluoromethyl)-1,3,5-triazin-2-amine

生成物 1

HCID 15008938HCID 15008938、化合物

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid溶媒HCID 887Methanol溶媒3 回HCID 962Water溶媒

実験手順

21.8 g of a 30% strength solution of sodium methanolate in methanol (0.12 mol of sodium methanolate) were added dropwise to a solution of 119.4 g (0.40 mol) of 2-methylamino-4-trichloromethyl-6-trifluoromethyl-1,3,5-triazine in 400 ml of methanol. The resulting yellow mixture was then refluxed for 1 hour during which it gradually became cloudy. After addition of a further 7.2 g of the 30% strength solution of sodium methanolate in methanol (0.04 mol of sodium methanolate), the mixture was refluxed for a further 30 minutes and, after cooling to 20° to 25° C., diluted with 150 ml of water and neutralized with 1 normal aqueous hydrochloric acid. The solvent was then removed at 40° C. under reduced pressure, after which the resulting solid was separated off and dried at 40° C. under reduced pressure for 15 hours.

後処理

  1. temperatureThe resulting yellow mixture was then refluxed for 1 hour during which it gradually became cloudy
  2. temperaturethe mixture was refluxed for a further 30 minutes
  3. temperatureafter cooling to 20° to 25° C.
  4. customThe solvent was then removed at 40° C. under reduced pressure
  5. customafter which the resulting solid was separated off
  6. customdried at 40° C. under reduced pressure for 15 hours

出典と根拠

ORDレコード
ord-412da58d239e4001a5a6c6a8595d92ff
出典データセット
uspto-grants-1992_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05130428

反応ノート

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