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Water → HCID 57629444、化合物

HRID 2108854
ノート
印刷プレビュー

反応式

HRID 2108854 の反応式
[CH2:1]([O:3][C:4]([C:6]1[CH:7]=[N:8][C:9]2[C:14]([C:15]=1[OH:16])=[CH:13][CH:12]=[C:11]([C:17]([F:20])([F:19])[F:18])[CH:10]=2)=[O:5])[CH3:2].C([O-])([O-])=O.[Cs+].[Cs+].Br[CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][O:33][C:34]1[C:35](=[O:42])[CH:36]=[C:37]([CH2:40][OH:41])[O:38][CH:39]=1.O>CN(C=O)C>[CH2:1]([O:3][C:4]([C:6]1[CH:7]=[N:8][C:9]2[C:14]([C:15]=1[O:16][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][O:33][C:34]1[C:35](=[O:42])[CH:36]=[C:37]([CH2:40][OH:41])[O:38][CH:39]=1)=[CH:13][CH:12]=[C:11]([C:17]([F:20])([F:18])[F:19])[CH:10]=2)=[O:5])[CH3:2]
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 4

HCID 962WaterHCID 10796Cesium carbonateHCID 179758375-(5-Bromopentyloxy)-2-(hydroxymethyl)-4H-pyran-4-oneHCID 178469560HCID 178469560、化合物

生成物 1

HCID 57629444HCID 57629444、化合物収率 31%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒
2 回

実験手順

4-Hydroxy-7-trifluoromethyl-quinoline-3-carboxylic acid ethyl ester (0.86 g, 3.02 mmol) was dissolved in DMF (10 mL). Cs2CO3 (0.98 g, 3.02 mmol) was added at RT and the mixture was stirred for 10 min. A solution of 5-(5-bromo-pentyloxy)-2-hydroxymethyl-pyran-4-one 10 (0.86 g, 3.02 mmol) in DMF (5 mL) was added via syringe. This mixture was stirred at 50° C. for 22 h. Water (10 mL) was added and the mixture extracted with EtOAc (2×50 mL), washed with water (3×50 mL), brine (3×50 mL) dried over MgSO4, filtered and evaporated. The crude product was purified by column chromatography on silica using as eluent (CH2Cl2:MeOH)=90:10. 4-[5-(6-Hydroxymethyl-4-oxo-4H-pyran-3-yloxy)-pentyloxy]-7-trifluoromethyl-quinoline-3-carboxylic acid ethyl ester 13 was obtained (0.43 g, 31% yield) as a pale yellow foam.

後処理

  1. stirringThis mixture was stirred at 50° C. for 22 h
  2. extractionthe mixture extracted with EtOAc (2×50 mL)
  3. washwashed with water (3×50 mL), brine (3×50 mL)
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customevaporated
  7. customThe crude product was purified by column chromatography on silica using as eluent (CH2Cl2:MeOH)=90:10

出典と根拠

ORDレコード
ord-a07bd55c87614e92be1e5d24a5f4608d
出典データセット
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07514432B2

反応ノート

読み込み中…

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