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Monobenzone → 3-[4-(Benzyloxy)phenoxy]-6-chloro-2-pyrazinecarbonitrile

HRID 392333
ノート
印刷プレビュー

反応式

HRID 392333 の反応式
Cl[C:2]1[C:3]([C:9]#[N:10])=[N:4][C:5]([Cl:8])=[CH:6][N:7]=1.[CH2:11]([O:18][C:19]1[CH:24]=[CH:23][C:22]([OH:25])=[CH:21][CH:20]=1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C(=O)([O-])[O-].[K+].[K+].C(OCC)(=O)C>CN(C)C=O.O>[CH2:11]([O:18][C:19]1[CH:20]=[CH:21][C:22]([O:25][C:2]2[C:3]([C:9]#[N:10])=[N:4][C:5]([Cl:8])=[CH:6][N:7]=2)=[CH:23][CH:24]=1)[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 7638MonobenzoneHCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 226628453,6-Dichloropyrazine-2-carbonitrile

生成物 1

HCID 226627883-[4-(Benzyloxy)phenoxy]-6-chloro-2-pyrazinecarbonitrile収率 79.1%

試薬・触媒・溶媒 2

HCID 962Water
溶媒
HCID 6228Dimethylformamide溶媒

実験手順

In 25 mL of dimethylformamide was dissolved 2.5 g of 3,6-dichloro-2-pyrazinecarbonitrile. After adding 3.2 g of 4-(benzyloxy)phenol and 3.0 g of potassium carbonate, the mixture was stirred at room temperature for one hour. A mixture of 25 ml of ethyl acetate and 100 mL of water was added to the reaction mixture, and the organic layer was separated. The organic layer thus obtained was washed successively with water and saturated aqueous solution of sodium chloride and dried on anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. Diisopropyl ether was added to the residue, the insoluble matter was filtered off, and the filtrate was concentrated. The residue thus obtained was washed with n-hexane to obtain 3.84 g of 3-[(4-(benzyloxy)phenoxy)]-6-chloro-2-pyrazinecarbonitrile as a light brown-colored solid product.

後処理

  1. additionwas added to the reaction mixture
  2. customthe organic layer was separated
  3. customThe organic layer thus obtained
  4. washwas washed successively with water and saturated aqueous solution of sodium chloride
  5. dry with materialdried on anhydrous magnesium sulfate
  6. customthe solvent was removed under reduced pressure
  7. additionDiisopropyl ether was added to the residue
  8. filtrationthe insoluble matter was filtered off
  9. concentrationthe filtrate was concentrated
  10. customThe residue thus obtained
  11. washwas washed with n-hexane

出典と根拠

ORDレコード
ord-6f1f6e73e2fc4e46b090e0eba055da6d
出典データセット
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06800629B2

反応ノート

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