Water → HCID 57210743, 화합물

HRID 2231975노트

반응식

HRID 2231975 반응식
[Cl:1][C:2]1[C:7]([C:8]#[N:9])=[C:6]([Cl:10])[C:5]([Cl:11])=[C:4](Cl)[C:3]=1[Cl:13].NCCNC(=O)[CH:19]([C:21]1[CH:26]=[C:25]([C:27]([CH3:30])([CH3:29])[CH3:28])[C:24]([OH:31])=[C:23]([C:32]([CH3:35])([CH3:34])[CH3:33])[CH:22]=1)[CH3:20].C([N:39](CC)CC)C.O.C[N:46]1[CH2:50][CH2:49]C[C:47]1=[O:51]>C1(C)C=CC=CC=1>[C:32]([C:23]1[CH:22]=[C:21]([CH2:19][CH2:20][C:47]([NH:46][CH2:50][CH2:49][NH:39][C:4]2[C:5]([Cl:11])=[C:6]([Cl:10])[C:7]([C:8]#[N:9])=[C:2]([Cl:1])[C:3]=2[Cl:13])=[O:51])[CH:26]=[C:25]([C:27]([CH3:30])([CH3:28])[CH3:29])[C:24]=1[OH:31])([CH3:35])([CH3:34])[CH3:33]

참가 물질

7

반응물 5

HCID 962WaterHCID 8471TriethylamineHCID 13387N-methyl-2-pyrrolidoneHCID 30363PentachlorobenzonitrileHCID 22104623HCID 22104623, 화합물

생성물 1

HCID 57210743HCID 57210743, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

27.6 g of pentachlorobenzonitrile and 32 g of 3,5-di-tert-butyl-4-hydroxyphenylpropionic acid 2-aminoethylamide are reacted with 11 g of triethylamine in 200 g of N-methylpyrrolidone for 7 hours at 100° C., after which 500 g of water and 400 g of toluene are added, and the toluene phase is separated off while still hot and evaporated down under reduced pressure. The residue is boiled with 0.15 l of ethanol, and the mixture is left to stand overnight at room temperature. The precipitate is then filtered off under suction and dried. After recrystallization from toluene, the product melts at 173°-175° C.

후처리

  1. customthe toluene phase is separated off while still hot and
  2. customevaporated down under reduced pressure
  3. waitthe mixture is left
  4. filtrationThe precipitate is then filtered off under suction
  5. customdried
  6. customAfter recrystallization from toluene

출처 및 근거

ORD 기록
ord-fa9c5be00d714278a88effefbf532837
출처 데이터셋
uspto-grants-1988_11
특허 번호
US04785107

반응 노트

불러오는 중…