1,2-Dichloroethane → HCID 13980725, 화합물

HRID 461309노트

반응식

HRID 461309 반응식
C([C:7]1[CH:12]=[CH:11][N:10]=[C:9]([C:13]2[CH:21]=[CH:20][C:16]([C:17]([NH2:19])=O)=[CH:15][CH:14]=2)[N:8]=1)CCCCC.[CH2:22](Cl)[CH2:23]Cl.P(Cl)(Cl)(Cl)=O>CCOCC>[CH2:9]([C:12]1[CH:11]=[N:10][C:9]([C:13]2[CH:14]=[CH:15][C:16]([C:17]#[N:19])=[CH:20][CH:21]=2)=[N:8][CH:7]=1)[CH2:13][CH2:14][CH2:15][CH2:22][CH3:23]

참가 물질

5

반응물 3

HCID 111,2-DichloroethaneHCID 24813Phosphorus oxychlorideHCID 541836714-(4-n-Hexylpyrimid-2-yl)benzoic acid amide

생성물 1

HCID 13980725HCID 13980725, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

15.58 g. of 4-(4-n-hexylpyrimid-2-yl)benzoic acid amide are left in a mixture of 350 ml. of ethylene chloride and 5.58 ml. of phosphorus oxychloride for 90 minutes under reflux, with stirring. The reaction mixture, diluted with ether, is washed with 2N sodium hydroxide solution and then with water until neutral. After evaporation of the organic phase, drying over sodium sulfate, 14.6 g. of 5-n-hexyl-2-(4-cyanophenyl)pyrimidine result, which are distilled in high vacuum, m.p. 53.5° - 54.5°; cl.p. 35.5° - 36.5°.

후처리

  1. washis washed with 2N sodium hydroxide solution
  2. customAfter evaporation of the organic phase
  3. dry with materialdrying over sodium sulfate, 14.6 g

출처 및 근거

ORD 기록
ord-37d61fc84d3a426d9c6824b870649a10
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04062798

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