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

HRID 2210364노트

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HRID 2210364 반응식
[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]

참가 물질

6

반응물 4

HCID 260Hydrogen BromideHCID 11430Potassium CarbonateHCID 60984Methyl bromoacetateHCID 19974138HCID 19974138, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d432a85120a44d1b940630548a152be8
출처 데이터셋
uspto-grants-1995_10
특허 번호
US05457205

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