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Sodium hydride → HCID 12056886、化合物

HRID 842568
ノート
印刷プレビュー

反応式

HRID 842568 の反応式
[Cl:1][C:2]1[CH:12]=[C:11]([O:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:10]=[C:9]([Cl:21])[C:3]=1[O:4][CH2:5][CH2:6][CH2:7][OH:8].[H-].[Na+].Cl[C:25]1[CH:30]=[CH:29][C:28]([C:31]([F:34])([F:33])[F:32])=[CH:27][N:26]=1>CN(C)C=O>[CH2:14]([O:13][C:11]1[CH:12]=[C:2]([Cl:1])[C:3]([O:4][CH2:5][CH2:6][CH2:7][O:8][C:25]2[CH:30]=[CH:29][C:28]([C:31]([F:34])([F:33])[F:32])=[CH:27][N:26]=2)=[C:9]([Cl:21])[CH:10]=1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 923422-Chloro-5-(trifluoromethyl)pyridineHCID 120568873-(2,6dichloro-4-(benzyloxy)phenoxy)-1-propyl alcohol

生成物 1

HCID 12056886HCID 12056886、化合物収率 69.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 0.5 g of 3-(2,6-dichloro-4-(benzyloxy)phenoxy)-1-propyl alcohol thus obtained, 0.1 g of an oily mixture containing 60% sodium hydride, and 3 ml of N,N-dimethylformamide was stirred at room temperature for 1 hour. Then, 0.3 g of 2-chloro-5-trifluoromethylpyridine was added to this mixture, followed by heating to 100° C. After stirring continued for 1 hour, the mixture was poured into 50 m of ice-water, and extracted with toluene at a total volume of 50 ml. The combined toluene layer was successively washed with diluted hydrochloric acid and aqueous sodium bicarbonate solution, dried with magnesium sulfate, and concentrated. The residue was silica gel chromatography, which afforded 0.5 g of 1-benzyloxy-3,5-dichloro-4-[3-(5-trifluoromethylpyridin-2-yloxy)propyloxy]benzene (67% yield).

後処理

  1. customthus obtained
  2. temperatureby heating to 100° C
  3. stirringAfter stirring
  4. waitcontinued for 1 hour
  5. extractionextracted with toluene at a total volume of 50 ml
  6. washThe combined toluene layer was successively washed with diluted hydrochloric acid and aqueous sodium bicarbonate solution
  7. dry with materialdried with magnesium sulfate
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-4dd43bc81c694c9f8784c3b5f78e3c27
出典データセット
uspto-grants-2002_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06376428B1

反応ノート

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