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Water → 7-Cyano-2-methoxy-1-naphthaldehyde

HRID 278041
ノート
印刷プレビュー

反応式

HRID 278041 の反応式
[C:1]([C:3]1[CH:12]=[CH:11][C:10]2[C:5](=[CH:6][C:7]([O:13][CH3:14])=[CH:8][CH:9]=2)[CH:4]=1)#[N:2].[CH3:15][O:16]C(Cl)Cl.O>ClCCl.[Ti](Cl)(Cl)(Cl)Cl>[C:1]([C:3]1[CH:4]=[C:5]2[C:10]([CH:9]=[CH:8][C:7]([O:13][CH3:14])=[C:6]2[CH:15]=[O:16])=[CH:11][CH:12]=1)#[N: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 3

HCID 962WaterHCID 21004Methane, dichloromethoxy-HCID 109541837-Methoxy-2-naphthonitrile

生成物 1

HCID 226276417-Cyano-2-methoxy-1-naphthaldehyde

試薬・触媒・溶媒 2

HCID 24193Titanium Tetrachloride触媒HCID 6344Dichloromethane溶媒

実験手順

Under nitrogen atmosphere, 3.7 g of 2-cyano-7-methoxynaphthalene was dissolved in 40 ml of dichloro- methane, and 6.6 ml of titanium tetrachloride and 4.6 ml of dichloromethyl methyl ether were added dropwise into the resulting solution at 0° in this order. The resulting mixture was stirred at room temperature for 30 minutes and cooled to 0° C. again. Water was added to the resulting mixture to cease the reaction, and the resulting mixture was extracted with dichloromethane (100 ml×2) The organic layers were combined, washed with water, a saturated aqueous solution of sodium bicarbonate and brine successively, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated and the resulting crude crystal was washed with ether and dried to give 3.3 g of the title compound as colorless crystals.

後処理

  1. temperaturecooled to 0° C. again
  2. customthe reaction
  3. extractionthe resulting mixture was extracted with dichloromethane (100 ml×2) The organic layers
  4. washwashed with water
  5. dry with materiala saturated aqueous solution of sodium bicarbonate and brine successively, dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated
  8. washthe resulting crude crystal was washed with ether
  9. customdried

出典と根拠

ORDレコード
ord-c1a6b8eb19d34939bde8829d030288c9
出典データセット
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06358995B1

反応ノート

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