Triethylamine → 4-(4-Morpholinylcarbonyl)phenyl trifluoromethanesulphonate

HRID 2179576ノート

反応式

HRID 2179576 の反応式
[F:1][C:2]([F:15])([F:14])[S:3]([O:6]S(C(F)(F)F)(=O)=O)(=[O:5])=[O:4].[N:16]1([C:22]([C:24]2[CH:29]=[CH:28][C:27](O)=[CH:26][CH:25]=2)=[O:23])[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1.C(N(CC)CC)C>ClCCl>[F:1][C:2]([F:15])([F:14])[S:3]([O:6][C:27]1[CH:26]=[CH:25][C:24]([C:22]([N:16]2[CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)=[O:23])=[CH:29][CH:28]=1)(=[O:5])=[O:4]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 67749Trifluoromethanesulfonic anhydrideHCID 7586556(4-Hydroxyphenyl)(morpholino)methanone

生成物 1

HCID 179828654-(4-Morpholinylcarbonyl)phenyl trifluoromethanesulphonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
-10 °C

実験手順

1.23 ml (7.24 mmol) of trifluoromethanesulphonic anhydride are slowly added dropwise to a solution, cooled to −10° C., of 1.0 g (4.83 mmol) of 4-(4-morpholinyl-carbonyl)phenol and 2.02 ml (14.48 mmol) of triethylamine in 20 ml of dichloromethane. The mixture is stirred at −10° C. for 30 min and then at 0° C. for 30 min. It is washed successively with 10% strength sodium bicarbonate solution, water and saturated sodium chloride solution, dried over sodium sulphate and concentrated in vacuo, and the residue is dried under high vacuum. 1.71 g (94.6% of theory) of the title compound are obtained.

後処理

  1. waitat 0° C. for 30 min
  2. washIt is washed successively with 10% strength sodium bicarbonate solution, water and saturated sodium chloride solution
  3. dry with materialdried over sodium sulphate
  4. concentrationconcentrated in vacuo
  5. customthe residue is dried under high vacuum

出典と根拠

ORDレコード
ord-66153291ff8e40ba9b726c9882f793e3
出典データセット
uspto-grants-2015_06
特許番号
US09067931B2

反応ノート

読み込み中…