4-Chlorobutyryl chloride → HCID 66620109, 화합물

HRID 415518노트

반응식

HRID 415518 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 66620109HCID 66620109, 화합물

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5f1d9f5421b444c0a23c14a28b7ac1db
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08088788B2

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