2-(3-Chloropropoxy)oxane → Formate

HRID 416510ノート

反応式

HRID 416510 の反応式
Cl[CH2:2][CH2:3][CH2:4][O:5][CH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][O:7]1.[CH:12]([N:15]1[CH2:20][CH2:19][CH:18]([NH:21][S:22]([CH2:25][CH2:26][NH:27][C:28]([C:30]2[S:31][C:32]([Cl:35])=[CH:33][CH:34]=2)=[O:29])(=[O:24])=[O:23])[CH2:17][CH2:16]1)([CH3:14])[CH3:13]>>[CH:12]([N:15]1[CH2:20][CH2:19][CH:18]([N:21]([CH2:2][CH2:3][CH2:4][O:5][CH:6]2[CH2:11][CH2:10][CH2:9][CH2:8][O:7]2)[S:22]([CH2:25][CH2:26][NH:27][C:28]([C:30]2[S:31][C:32]([Cl:35])=[CH:33][CH:34]=2)=[O:29])(=[O:23])=[O:24])[CH2:17][CH2:16]1)([CH3:14])[CH3:13].[CH:6]([O-:7])=[O:5]

参加物

4

反応物 2

HCID 2549542-(3-Chloropropoxy)oxaneHCID 119904785-Chloro-Thiophene-2-Carboxylic Acid [2-(1--Isopropyl-Piperidin-4-Ylsulfamoyl)-Ethyl]-Amide

生成物 2

HCID 283FormateHCID 666249655-Chloro-thiophene-2-carboxylic acid (2-{(1-isopropyl-piperidin-4-yl)-[3-(tetrahydro-pyran-2-yloxy)-propyl]-sulfamoyl}-ethyl)-amide

実験手順

5-Chloro-thiophene-2-carboxylic acid (2-{(1-isopropyl-piperidin-4-yl)-[3-(tetrahydro-pyran-2-yloxy)-propyl]-sulfamoyl}-ethyl)-amide was prepared by an analogous procedure as described in example 15 starting from 245 mg (1.5 equiv.) 2-(3-chloro-propoxy)-tetrahydro-pyran and 360 mg (0.91 mmol) 5-chloro-thiophene-2-carboxylic acid [2-(1-isopropyl-piperidin-4-ylsulfamoyl)-ethyl]-amide. Final purification by preparative RP-HPLC (CH3CN/H2O gradient+0.05% formic acid) gave pure 5-chloro-thiophene-2-carboxylic acid (2-{(1-isopropyl-piperidin-4-yl)-[3-(tetrahydro-pyran-2-yloxy)-propyl]-sulfamoyl}-ethyl)-amide as its formate.

後処理

  1. custom5-Chloro-thiophene-2-carboxylic acid (2-{(1-isopropyl-piperidin-4-yl)-[3-(tetrahydro-pyran-2-yloxy)-propyl]-sulfamoyl}-ethyl)-amide was prepared by an analogous procedure
  2. customFinal purification by preparative RP-HPLC (CH3CN/H2O gradient+0.05% formic acid)

出典と根拠

ORDレコード
ord-1b71ff41d8d248618cbc5a65721d9f28
出典データセット
uspto-grants-2012_01
特許番号
US08088925B2

反応ノート

読み込み中…