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Benzoyl chloride → HCID 13406007、化合物

HRID 1179668
ノート
印刷プレビュー

反応式

HRID 1179668 の反応式
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([O:8][CH3:9])=[N:6][CH:7]=1.C(N(C(C)C)C(C)C)C.[C:19](Cl)(=[O:26])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.CCCCCCC>ClCCl>[CH3:9][O:8][C:5]1[N:6]=[CH:7][C:2]([NH:1][C:19](=[O:26])[C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[CH:3][CH:4]=1
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 7412Benzoyl chlorideHCID 8900HeptaneHCID 811216-Methoxy-3-pyridinylamineHCID 81531Diisopropylethylamine

生成物 1

HCID 13406007HCID 13406007、化合物収率 75.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 5-amino-2-methoxypyridine (2.48 g, 20.0 mmol) and N-ethyldiisopropylamine (2.84 g, 22.0 mmol) in dichloromethane (20 ml) was cooled in an ice-bath. Benzoyl chloride (3.09 g, 22 mmol) was slowly added by means of a syringe. The cooling bath was removed and stirring was continued at room temperature for 18 hours. Dichloromethane was added and the solution was extracted with water. The organic layer was dried over sodium sulphate, filtered and evaporated in vacuo leaving a dark solid. Crystallisation from ethyl acetate:heptane yielded the title compound (3.44 g, 75% yield).

後処理

  1. customThe cooling bath was removed
  2. additionDichloromethane was added
  3. extractionthe solution was extracted with water
  4. dry with materialThe organic layer was dried over sodium sulphate
  5. filtrationfiltered
  6. customevaporated in vacuo
  7. customleaving a dark solid
  8. customCrystallisation from ethyl acetate

出典と根拠

ORDレコード
ord-dcf8f02b306b4720978b3a3744336821
出典データセット
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07279470B2

反応ノート

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