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

Sodium Hydroxide → 3-Amino-6-fluoro-2-(2'-fluoro[1,1'-biphenyl]-4-yl)-4-quinolinecarboxylic acid

HRID 1073263
ノート
印刷プレビュー

反応式

HRID 1073263 の反応式
[F:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][C:6](=[O:11])[C:5]2=O.[OH-:13].[Na+].Cl.[NH2:16][CH2:17][C:18]([C:20]1[CH:25]=[CH:24][C:23]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=2[F:32])=[CH:22][CH:21]=1)=O>O.C(O)C.O.O1CCCC1>[NH2:16][C:17]1[C:18]([C:20]2[CH:25]=[CH:24][C:23]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=3[F:32])=[CH:22][CH:21]=2)=[N:7][C:8]2[C:4]([C:5]=1[C:6]([OH:11])=[O:13])=[CH:3][C:2]([F:1])=[CH:10][CH:9]=2
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 14798Sodium HydroxideHCID 2365665-FluoroisatinHCID 221583512-Amino-1-(2'-fluoro[1,1'-biphenyl]-4-yl)-ethanone hydrochloride

生成物 1

HCID 150859603-Amino-6-fluoro-2-(2'-fluoro[1,1'-biphenyl]-4-yl)-4-quinolinecarboxylic acid収率 79.1%

試薬・触媒・溶媒 3

HCID 962Water溶媒2 回
HCID 8028
Tetrahydrofuran
溶媒
HCID 19096565Water ethanol溶媒

実験手順

To a stirred suspension of 4.13 g of 5-fluoroisatin in 40 ml of water was added a solution of 5.62 g of sodium hydroxide in 20 ml of water. This mixture was heated to 85°-90° C. and a warm solution of 9.3 g of 2-amino-1 (2'-fluoro[1,1'-biphenyl]-4-yl)ethanone, hydrochloride in 140 ml of ethanol:water (1:1) and 30 ml of tetrahydrofuran was added dropwise over 2 hours. This mixture was stirred at reflux for 2 hours, then the ethanol was distilled off. The reaction was filtered and the filtrate acidified to pH 4-5 with acetic acid. The resulting solid was collected, washed with water and crystallized from 400 ml of hot ethanol, giving 7.45 g of the desired product as a yellow solid, mp 248°-250° C.

後処理

  1. temperatureThis mixture was heated to 85°-90° C.
  2. temperatureat reflux for 2 hours
  3. distillationthe ethanol was distilled off
  4. filtrationThe reaction was filtered
  5. customThe resulting solid was collected
  6. washwashed with water
  7. customcrystallized from 400 ml of hot ethanol

出典と根拠

ORDレコード
ord-95395aac5bb04592a69a49f71bcafa53
出典データセット
uspto-grants-1990_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04968702

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート