4-Chlorobutyryl chloride → HCID 66620109、化合物

HRID 415518ノート

反応式

HRID 415518 の反応式
[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][N:10]=2)[N:5]=[CH:4][C:3]=1[NH2:12].[Cl:13][CH2:14][CH2:15][CH2:16][C:17](Cl)=[O:18]>ClCCCl>[Cl:13][CH2:14][CH2:15][CH2:16][C:17]([NH:12][C:3]1[CH:4]=[N:5][C:6]2[C:11]([C:2]=1[Cl:1])=[N:10][CH:9]=[CH:8][CH:7]=2)=[O:18]

参加物

4

反応物 2

HCID 783704-Chlorobutyryl chlorideHCID 666199614-Chloro-1,5-naphthyridin-3-amine

生成物 1

HCID 66620109HCID 66620109、化合物

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

A mixture of 4-chloro[1,5]naphthyridin-3-amine (2.0 g, 11 mmol) and 4-chlorobutyryl chloride (4.7 g, 33 mmol) in 1,2-dichloroethane (75 mL) was heated at reflux for 20 hours. The reaction mixture was then concentrated under reduced pressure and the residue washed with two 25 mL portions of hexane. The solid was then taken up in methanol (35 mL), 1.0 mL of 10% solution of sodium hydroxide in water was added, and the solution was stirred at room temperature for 4 hours. The reaction mixture was then concentrated under reduced pressure to provide 4-chloro-N-(4-chloro[1,5]naphthyridin-3-yl)butanamide which was used directly in the next step without further purification.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 20 hours
  3. concentrationThe reaction mixture was then concentrated under reduced pressure
  4. washthe residue washed with two 25 mL portions of hexane
  5. addition1.0 mL of 10% solution of sodium hydroxide in water was added
  6. concentrationThe reaction mixture was then concentrated under reduced pressure

出典と根拠

ORDレコード
ord-5f1d9f5421b444c0a23c14a28b7ac1db
出典データセット
uspto-grants-2012_01
特許番号
US08088788B2

反応ノート

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