Water → HCID 57069684, 화합물

HRID 2231977노트

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HRID 2231977 반응식
[Cl:1][C:2]1[N:9]=[C:8](Cl)[CH:7]=[C:6]([CH3:11])[C:3]=1[C:4]#[N:5].NCCNC(=O)[CH:17]([C:19]1[CH:24]=[C:23]([C:25]([CH3:28])([CH3:27])[CH3:26])[C:22]([OH:29])=[C:21]([C:30]([CH3:33])([CH3:32])[CH3:31])[CH:20]=1)[CH3:18].C([N:37](CC)CC)C.O.C[N:44]1[CH2:48][CH2:47]C[C:45]1=[O:49]>C1(C)C=CC=CC=1>[C:30]([C:21]1[CH:20]=[C:19]([CH2:17][CH2:18][C:45]([NH:44][CH2:48][CH2:47][NH:37][C:8]2[CH:7]=[C:6]([CH3:11])[C:3]([C:4]#[N:5])=[C:2]([Cl:1])[N:9]=2)=[O:49])[CH:24]=[C:23]([C:25]([CH3:28])([CH3:26])[CH3:27])[C:22]=1[OH:29])([CH3:33])([CH3:32])[CH3:31]

참가 물질

7

반응물 5

HCID 962WaterHCID 8471TriethylamineHCID 13387N-methyl-2-pyrrolidoneHCID 701313-Cyano-2,6-dichloro-4-methylpyridineHCID 22104623HCID 22104623, 화합물

생성물 1

HCID 57069684HCID 57069684, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

18.7 g of 2,6-dichloro-4-methylnicotinonitrile and 32 g of 3,5-di-tert-butyl-4-hydroxyphenylpropionic acid 2-aminoethylamide are reacted with 10.1 g of triethylamine in 0.2 l of N-methylpyrrolidone at 50° C. for 8 hours, after which 1 l of water and 0.4 l of toluene are added, the toluene phase is separated off, dried and filtered over active carbon, and the filtrate is evaporated down. The residue is dissolved in 100 ml of hot ethanol, and 1 l of petroleum ether is slowly added to the solution. The mixture is cooled, and the precipitate is filtered off under suction and dried to give a product of melting point 162°-165° C.

후처리

  1. customthe toluene phase is separated off
  2. customdried
  3. filtrationfiltered over active carbon
  4. customthe filtrate is evaporated down
  5. dissolutionThe residue is dissolved in 100 ml of hot ethanol
  6. addition1 l of petroleum ether is slowly added to the solution
  7. temperatureThe mixture is cooled
  8. filtrationthe precipitate is filtered off under suction
  9. customdried
  10. customto give a product of melting point 162°-165° C.

출처 및 근거

ORD 기록
ord-23c2844a1e964804a3e1820609c83d29
출처 데이터셋
uspto-grants-1988_11
특허 번호
US04785107

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