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

Lithium hydroxide, monohydrate → 5-{[2-(4-Carboxyphenyl)ethyl][2-(2-{[4-(5-chloro-1,3-benzoxazol-2-yl)benzyl]oxy}phenyl)ethyl]-amino}-5,6,7,8-tetrahydroquinoline-2-carboxylic acid

HRID 875355
ノート
印刷プレビュー

反応式

HRID 875355 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][C:8]([C:10]3[CH:53]=[CH:52][C:13]([CH2:14][O:15][C:16]4[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=4[CH2:22][CH2:23][N:24]([CH2:40][CH2:41][C:42]4[CH:47]=[CH:46][C:45]([C:48]([O:50]C)=[O:49])=[CH:44][CH:43]=4)[CH:25]4[CH2:34][CH2:33][CH2:32][C:31]5[N:30]=[C:29]([C:35]([O:37]CC)=[O:36])[CH:28]=[CH:27][C:26]4=5)=[CH:12][CH:11]=3)=[N:7][C:6]=2[CH:54]=1.O.[OH-].[Li+]>C1COCC1.O>[C:48]([C:45]1[CH:46]=[CH:47][C:42]([CH2:41][CH2:40][N:24]([CH2:23][CH2:22][C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=2[O:15][CH2:14][C:13]2[CH:12]=[CH:11][C:10]([C:8]3[O:9][C:5]4[CH:4]=[CH:3][C:2]([Cl:1])=[CH:54][C:6]=4[N:7]=3)=[CH:53][CH:52]=2)[CH:25]2[CH2:34][CH2:33][CH2:32][C:31]3[N:30]=[C:29]([C:35]([OH:37])=[O:36])[CH:28]=[CH:27][C:26]2=3)=[CH:43][CH:44]=1)([OH:50])=[O:49]
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

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 86709810Ethyl 5-([2-(2-{[4-(5-chloro-1,3-benzoxazol-2-yl)benzyl]oxy}phenyl)ethyl]{2-[4-(methoxy-carbonyl)phenyl]ethyl}amino)-5,6,7,8-tetrahydroquinoline-2-carboxylate

生成物 1

HCID 730577385-{[2-(4-Carboxyphenyl)ethyl][2-(2-{[4-(5-chloro-1,3-benzoxazol-2-yl)benzyl]oxy}phenyl)ethyl]-amino}-5,6,7,8-tetrahydroquinoline-2-carboxylic acid

試薬・触媒・溶媒 2

HCID 962Water
溶媒
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

68 mg (0.09 mmol) of ethyl 5-([2-(2-{[4-(5-chloro-1,3-benzoxazol-2-yl)benzyl]oxy}-phenyl)ethyl]-{2-[4-(methoxycarbonyl)phenyl]ethyl}amino)-5,6,7,8-tetrahydroquinoline-2-carboxylate (Enantiomer 1, Example 63A) were taken up in 4 ml of THF and 2 ml of water, and 12 mg (0.27 mmol) of lithium hydroxide monohydrate were added. The reaction was stirred at 60° C. overnight. After the reaction had gone to completion, the THF was removed on a rotary evaporator and the mixture that remained was diluted with water. The mixture was then acidified to pH 4-5 using acetic acid and extracted repeatedly with ethyl acetate. The combined organic phases were dried over magnesium sulphate, filtered and concentrated to dryness. This gave 33 mg (0.04 mmol, 48% of theory) of the title compound.

後処理

  1. customthe THF was removed on a rotary evaporator
  2. additionthe mixture that remained was diluted with water
  3. extractionextracted repeatedly with ethyl acetate
  4. dry with materialThe combined organic phases were dried over magnesium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-b68dbf2ae902440096c6c4c3743dae85
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08981104B2

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