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Cesium carbonate → 4-{2-[(4-Benzyloxycarbonyl methoxy-7-methyl-quinoline-2-carbonyl)-amino]-acetyl}-piperazine-1-carboxylic acid butyl ester

HRID 1185490
ノート
印刷プレビュー

反応式

HRID 1185490 の反応式
[CH2:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14](=[O:31])[CH2:15][NH:16][C:17]([C:19]2[CH:28]=[C:27](O)[C:26]3[C:21](=[CH:22][C:23]([CH3:30])=[CH:24][CH:25]=3)[N:20]=2)=[O:18])[CH2:10][CH2:9]1)=[O:7])[CH2:2][CH2:3][CH3:4].[C:32](=O)([O-])[O-:33].[Cs+].[Cs+].[CH2:38]([O:45][C:46](=[O:49])CBr)[C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1>CN(C=O)C.O>[CH2:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14](=[O:31])[CH2:15][NH:16][C:17]([C:19]2[C:28]([O:33][CH3:32])=[C:27]([C:46]([O:45][CH2:38][C:39]3[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=3)=[O:49])[C:26]3[C:21](=[CH:22][C:23]([CH3:30])=[CH:24][CH:25]=3)[N:20]=2)=[O:18])[CH2:10][CH2:9]1)=[O:7])[CH2:2][CH2:3][CH3:4]
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 62576Benzyl bromoacetateHCID 178452377HCID 178452377、化合物

生成物 1

HCID 686001674-{2-[(4-Benzyloxycarbonyl methoxy-7-methyl-quinoline-2-carbonyl)-amino]-acetyl}-piperazine-1-carboxylic acid butyl ester

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6228
Dimethylformamide
溶媒

実験手順

To a solution of 4.5 g 4-{2-[(4-Hydroxy-7-methyl-quinoline-2-carbonyl)-amino]-acetyl}-piperazine-1-carboxylic acid butyl ester in 30 ml of DMF, 3.7 g of cesium carbonate and 2.6 g of Bromo-acetic acid benzyl ester were added and the reaction mixture was stirred for 16 h at RT. Then, the reaction mixture was diluted with water and extracted with ethyl acetate. The organic phase was dried over MgSO4 and the solvents were removed under reduced pressure. The isolated crude product was purified by re-crystallising from ethyl acetate/heptane. Yield: 5 g.

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic phase was dried over MgSO4
  3. customthe solvents were removed under reduced pressure
  4. customThe isolated crude product
  5. customwas purified
  6. customby re-crystallising from ethyl acetate/heptane

出典と根拠

ORDレコード
ord-7878b00750664dac8080ab4b0ace3352
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08669266B2

反応ノート

読み込み中…

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