Potassium Carbonate → [2-(3-Thieno[2,3-d]isoxazol-3-yl-phenoxy)-ethyl]-(2-trifluoromethylbenzyl)-amine

HRID 8667

反応式

HRID 8667 の反応式
Br[CH2:2][CH2:3][O:4][C:5]1[CH:6]=[C:7]([C:11]2[C:15]3[S:16][CH:17]=[CH:18][C:14]=3[O:13][N:12]=2)[CH:8]=[CH:9][CH:10]=1.C(=O)([O-])[O-].[K+].[K+].[F:25][C:26]([F:36])([F:35])[C:27]1[CH:34]=[CH:33][CH:32]=[CH:31][C:28]=1[CH2:29][NH2:30]>C(#N)C>[O:13]1[C:14]2[CH:18]=[CH:17][S:16][C:15]=2[C:11]([C:7]2[CH:6]=[C:5]([CH:10]=[CH:9][CH:8]=2)[O:4][CH2:3][CH2:2][NH:30][CH2:29][C:28]2[CH:31]=[CH:32][CH:33]=[CH:34][C:27]=2[C:26]([F:25])([F:35])[F:36])=[N:12]1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 764472-(Trifluoromethyl)benzylamineHCID 219835823-[3-(2-Bromo-ethoxy)-phenyl]-thieno[2,3-d]isoxazole

生成物 1

HCID 21983566[2-(3-Thieno[2,3-d]isoxazol-3-yl-phenoxy)-ethyl]-(2-trifluoromethylbenzyl)-amine収率 96.4%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

The title compound is prepared from 3-[3-(2-bromo-ethoxy)-phenyl]-thieno[2,3-d]isoxazole (0.250 g, 0.771 mmol), potassium carbonate (0.205 g, 1.48 mmol), 2-(trifluoromethyl)benzylamine (0.676 mg, 3.86 mmol) and acetonitrile (4 mL) essentially as described above in example 18 except that the reaction is run overnight and the compound is purified by column using a solvent gradient of 5% ethyl acetate in dichloromethane to 10% methanol in ethyl acetate to give the title compound (0.311 g, 96% Yield). Purity by LC/MS (APCI)=99%, [M+H]+=419.

後処理

  1. customthe compound is purified by column

出典と根拠

ORDレコード
ord-7425231cb5054edb8397a2b558164d3f
出典データセット
uspto-grants-2006_08
特許番号
US07091199B1

関連ノート

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