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2,2,2-Trifluoroethanol → Stk076603

HRID 1252645
ノート
印刷プレビュー

反応式

HRID 1252645 の反応式
[NH2:1][C:2]1[N:7]=[C:6](Cl)[N:5]=[C:4]([NH:9][CH3:10])[N:3]=1.[OH-].[K+].[F:13][C:14]([F:18])([F:17])[CH2:15][OH:16]>>[NH2:1][C:2]1[N:3]=[C:4]([NH:9][CH3:10])[N:5]=[C:6]([O:16][CH2:15][C:14]([F:18])([F:17])[F:13])[N:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 64092,2,2-TrifluoroethanolHCID 14797Potassium HydroxideHCID 2249702-Chloro-4-methylamino-6-amino-1,3,5-triazine-

生成物 1

HCID 1375559Stk076603

実験手順

2-Amino-4-chloro-6-methylamino-1,3,5-triazine (0.2 mole) was slurried in 80 ml of 2,2,2-trifluoroethanol at room temperature. Potassium hydroxide pellets (0.2 mole) were added portionwise and the mixture was stirred at room temperature overnight. The following day the reaction was heated at gentle reflux for 2 hours during which time the solids gradually dissolved. The solution was cooled and the solvent was removed under vacuum. The residue was washed with water and filtered to give 20.9 g shining off-white crystals of the product named above with the following characteristics: m.p. 204°-205° C. NMR (DMSO-d6): δ 2.75, d, (NHCH3); 4.8, q, (OCH2CF3); 6.5-7.3, m, (NH2 +NHCH3).

後処理

  1. temperatureThe following day the reaction was heated
  2. temperatureat gentle reflux for 2 hours during which time the solids
  3. dissolutiongradually dissolved
  4. temperatureThe solution was cooled
  5. customthe solvent was removed under vacuum
  6. washThe residue was washed with water
  7. filtrationfiltered
  8. customto give 20.9 g

出典と根拠

ORDレコード
ord-d712683cafd14d8a9eacbbb8c7af22db
出典データセット
uspto-grants-1988_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04744816

反応ノート

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