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Cesium carbonate → 2-Chloro-N-(1-hydroxy-cycloheptylmethyl)-5-[4-(2-methoxy-ethyl)-5-oxo-4,5-dihydro-[1,2,4]triazol-1-yl]-benzamide

HRID 1790283
ノート
印刷プレビュー

反応式

HRID 1790283 の反応式
[Cl:1][C:2]1[CH:19]=[CH:18][C:17]([N:20]2[C:24](=[O:25])[NH:23][CH:22]=[N:21]2)=[CH:16][C:3]=1[C:4]([NH:6][CH2:7][C:8]1([OH:15])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1)=[O:5].C([O-])([O-])=O.[Cs+].[Cs+].[CH3:32][O:33][CH2:34][CH2:35]Br>CS(C)=O.O>[Cl:1][C:2]1[CH:19]=[CH:18][C:17]([N:20]2[C:24](=[O:25])[N:23]([CH2:35][CH2:34][O:33][CH3:32])[CH:22]=[N:21]2)=[CH:16][C:3]=1[C:4]([NH:6][CH2:7][C:8]1([OH:15])[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14]1)=[O:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 10796Cesium carbonateHCID 809722-Bromoethyl methyl etherHCID 135492557HCID 135492557、化合物

生成物 1

HCID 99320472-Chloro-N-(1-hydroxy-cycloheptylmethyl)-5-[4-(2-methoxy-ethyl)-5-oxo-4,5-dihydro-[1,2,4]triazol-1-yl]-benzamide収率 34.9%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒
HCID 962
Water
溶媒

実験手順

A slurry of 2-Chloro-N-(1-hydroxy-cycloheptylmethyl)-5-(5-oxo-4,5-dihydro-[1,2,4]triazol-1-yl)-benzamide (44.4 mg, 0.122 mmol) and Cs2CO3 (66.0 mg, 0.202 mmol) were stirred in DMSO (0.813 mL) at ambient temperature for 20 minutes. 2-Bromoethyl methyl ether (17.0 mg, 0.122 mmol) was added and the reaction stirred at ambient temperature for 48 hours. The reaction was diluted with water (15-fold) and the aqueous extracted with CH2Cl2 (3×). The organics were dried over sodium sulfate, and concentrated in vacuo. The crude was purified by reverse phase HPLC reverse phase HPLC using a (25–65% gradient of 0.1% formic acid in acetonitrile and 0.1% formic acid in water) (to give the title compound (18 mg). LCMS (m/z) 423.5 M+1.

後処理

  1. extractionthe aqueous extracted with CH2Cl2 (3×)
  2. dry with materialThe organics were dried over sodium sulfate
  3. concentrationconcentrated in vacuo
  4. customThe crude was purified by reverse phase HPLC reverse phase HPLC

出典と根拠

ORDレコード
ord-d7b0d0dd863f4f7a88433015679f4e3f
出典データセット
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07071223B1

反応ノート

読み込み中…

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