Hydrogen Bromide → N-[2-(4-Carbomethoxymethoxyphenyl)ethyl]-2-(2-trifluoromethyl-thiazol-4-yl)morpholine

HRID 1451433ノート

反応式

HRID 1451433 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][N:11]2[CH2:16][CH2:15][O:14][CH:13]([C:17]3[N:18]=[C:19]([C:22]([F:25])([F:24])[F:23])[S:20][CH:21]=3)[CH2:12]2)=[CH:5][CH:4]=1.Br.C(=O)([O-])[O-].[K+].[K+].BrC[C:35]([O:37][CH3:38])=[O:36]>CC(C)=O>[C:35]([CH2:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][N:11]2[CH2:16][CH2:15][O:14][CH:13]([C:17]3[N:18]=[C:19]([C:22]([F:25])([F:24])[F:23])[S:20][CH:21]=3)[CH2:12]2)=[CH:5][CH:4]=1)([O:37][CH3:38])=[O:36]

参加物

6

反応物 4

HCID 260Hydrogen BromideHCID 11430Potassium CarbonateHCID 60984Methyl bromoacetateHCID 19974138HCID 19974138、化合物

生成物 1

HCID 19974221N-[2-(4-Carbomethoxymethoxyphenyl)ethyl]-2-(2-trifluoromethyl-thiazol-4-yl)morpholine

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

0.6 g (1.6 mmol) of N-[2-(4-Methoxyphenyl)ethyl]-2-(2-trifluoromethyl-thiazol-4-yl)morpholine are heated on a steam bath with 6 ml of 48% strength aqueous hydrobromic acid for 3 hours. The mixture is then concentrated, toluene is added, and the mixture is again evaporated to dryness. The foamy residue is boiled under reflux in 15 ml of acetone with 1.2 g (8.7 mmol) of potassium carbonate and 0.3 ml (1.65 mmol) of methyl bromoacetate for 1 hour. The mixture is then filtered, the filtrate is concentrated, and the residue is purified on a silica gel column using toluene/acetone=4:1.

後処理

  1. concentrationThe mixture is then concentrated
  2. additiontoluene is added
  3. customthe mixture is again evaporated to dryness
  4. filtrationThe mixture is then filtered
  5. concentrationthe filtrate is concentrated
  6. customthe residue is purified on a silica gel column

出典と根拠

ORDレコード
ord-39bc7ba453a444ef92c1287ff9c3a27f
出典データセット
uspto-grants-1997_02
特許番号
US05604225

反応ノート

読み込み中…