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Lithium Hydroxide → 6-(6-(3-Ethylureido)-4-(4-(trifluoromethyl)thiazol-2-yl)pyridin-3-yl)-1-(2-methoxyethyl)-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

HRID 2061800
ノート
印刷プレビュー

反応式

HRID 2061800 の反応式
[CH2:1]([NH:3][C:4](=[O:41])[NH:5][C:6]1[N:11]=[CH:10][C:9]([C:12]2[CH:13]=[C:14]3[C:19](=[CH:20][CH:21]=2)[N:18]([CH2:22][CH2:23][O:24][CH3:25])[CH:17]=[C:16]([C:26]([O:28]CC)=[O:27])[C:15]3=[O:31])=[C:8]([C:32]2[S:33][CH:34]=[C:35]([C:37]([F:40])([F:39])[F:38])[N:36]=2)[CH:7]=1)[CH3:2].[Li+].[OH-].C1COCC1>CO.O>[CH2:1]([NH:3][C:4](=[O:41])[NH:5][C:6]1[N:11]=[CH:10][C:9]([C:12]2[CH:13]=[C:14]3[C:19](=[CH:20][CH:21]=2)[N:18]([CH2:22][CH2:23][O:24][CH3:25])[CH:17]=[C:16]([C:26]([OH:28])=[O:27])[C:15]3=[O:31])=[C:8]([C:32]2[S:33][CH:34]=[C:35]([C:37]([F:39])([F:40])[F:38])[N:36]=2)[CH:7]=1)[CH3:2]
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

6

反応物 3

HCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 59416012Ethyl 6-(6-(3-ethylureido)-4-(4-(trifluoromethyl)thiazol-2-yl)pyridin-3-yl)-1-(2-methoxyethyl)-4-oxo-1,4-dihydroquinoline-3-carboxylate

生成物 1

HCID 445401686-(6-(3-Ethylureido)-4-(4-(trifluoromethyl)thiazol-2-yl)pyridin-3-yl)-1-(2-methoxyethyl)-4-oxo-1,4-dihydroquinoline-3-carboxylic acid収率 74.8%

試薬・触媒・溶媒 2

HCID 887
Methanol
溶媒
HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

Ethyl 6-(6-(3-ethylureido)-4-(4-(trifluoromethyl)thiazol-2-yl)pyridin-3-yl)-1-(2-methoxyethyl)-4-oxo-1,4-dihydroquinoline-3-carboxylate (Example 51, 0.090 g, 0.15 mmol) and LiOH (0.092 mL, 0.18 mmol) were combined in MeOH (1 mL)/THF (1 mL) and heated to 100° C. in the microwave for 15 min The reaction mixture was cooled to room temperature, diluted with water (1.000 mL) and heated until the compound dissolved. The resulting solution was filtered and the filtrate was then concentrated under reduced pressure to remove methanol. HCl (1 N) was added and the resulting precipitate was collected by filtration, washed with water and dried overnight to yield a white solid (0.063 g).

後処理

  1. temperaturewas cooled to room temperature
  2. temperatureheated until the compound
  3. dissolutiondissolved
  4. filtrationThe resulting solution was filtered
  5. concentrationthe filtrate was then concentrated under reduced pressure
  6. customto remove methanol. HCl (1 N)
  7. additionwas added
  8. filtrationthe resulting precipitate was collected by filtration
  9. washwashed with water
  10. customdried overnight

出典と根拠

ORDレコード
ord-2319054b025646a2bca36bc19a6f8f4a
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08283361B2

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