ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Water → HCID 18979554、化合物

HRID 2392587
ノート
印刷プレビュー

反応式

HRID 2392587 の反応式
C([N:3]([CH2:6][CH3:7])CC)C.CS(Cl)(=O)=O.[C:13]([O:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][O:26][C:27]1[CH:32]=[CH:31][C:30]([C:33]2[CH:38]=[CH:37][C:36]([C:39]([OH:41])=[O:40])=[CH:35][CH:34]=2)=[CH:29][CH:28]=1)(=[O:16])[CH:14]=[CH2:15].O[C:43]1[CH:44]=[C:45]([CH:48]=[CH:49][C:50]=1[OH:51])[C:46]#N.[OH2:52]>O1CCCC1.CN(C)C1C=CN=CC=1>[C:13]([O:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][O:26][C:27]1[CH:28]=[CH:29][C:30]([C:33]2[CH:38]=[CH:37][C:36]([C:39]([O:41][C:28]3[CH:29]=[C:7]([CH:31]=[CH:32][C:27]=3[O:52][C:39]([C:36]3[CH:37]=[CH:38][C:46]([C:45]4[CH:48]=[CH:49][C:50]([O:51][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][O:17][C:13](=[O:16])[CH:14]=[CH2:15])=[CH:43][CH:44]=4)=[CH:34][CH:35]=3)=[O:40])[C:6]#[N:3])=[O:40])=[CH:35][CH:34]=2)=[CH:31][CH:32]=1)(=[O:16])[CH:14]=[CH2:15]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 870653,4-DihydroxybenzonitrileHCID 18979499HCID 18979499、化合物

生成物 1

HCID 18979554HCID 18979554、化合物

試薬・触媒・溶媒 2

HCID 14284
4-(Dimethylamino)pyridine
触媒
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-25 °C

実験手順

0.9 g of triethylamine and then 0.5 g of methanesulphonyl chloride were added dropwise at -25° C. while stirring to a solution of 2.0 g of 4-(8-acryloyloxyoctyloxy)biphenyl-4'-carboxylic acid in 40 ml of tetrahydrofuran. The reaction mixture was stirred at -25° C. for 1 hour, then treated with 0.25 g of 3,4-dihydroxybenzonitrile and 0.05 g of 4-(dimethylamino)pyridine, stirred at room temperature overnight, poured into 100 ml of water and then extracted three times with 50 ml of diethyl ether each time. The organic phases were combined, washed twice with 100 ml of water each time, dried over magnesium sulphate, filtered and the filtrate was concentrated. Chromatographic purification of the residue on silica gel with cyclohexane/ethyl acetate (vol. 8:2) and two-fold recrystallization from a cyclohexane/ethyl acetate mixture (vol. 8:2) of the fractions which were pure according to thin-layer chromatography gave 1.0 g of 3,4-bis[4-(8-acryloyloxyoctyloxy)biphenyl-4'-carbonyloxy]benzonitrile.

後処理

  1. stirringstirred at room temperature overnight
  2. extractionextracted three times with 50 ml of diethyl ether each time
  3. washwashed twice with 100 ml of water each time
  4. dry with materialdried over magnesium sulphate
  5. filtrationfiltered
  6. concentrationthe filtrate was concentrated
  7. customChromatographic purification of the residue on silica gel
  8. customwith cyclohexane/ethyl acetate (vol. 8:2) and two-fold recrystallization from a cyclohexane/ethyl acetate mixture (vol. 8:2) of the fractions which

出典と根拠

ORDレコード
ord-bcec63a8d5c540ef94a9d2d0399c143b
出典データセット
uspto-grants-1998_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05800733

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート