Water → HCID 57210743、化合物

HRID 2231975ノート

反応式

HRID 2231975 の反応式
[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]

参加物

7

反応物 5

HCID 962WaterHCID 8471TriethylamineHCID 13387N-methyl-2-pyrrolidoneHCID 30363PentachlorobenzonitrileHCID 22104623HCID 22104623、化合物

生成物 1

HCID 57210743HCID 57210743、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fa9c5be00d714278a88effefbf532837
出典データセット
uspto-grants-1988_11
特許番号
US04785107

反応ノート

読み込み中…