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 → 2-[2-(4-{2-[Ethyl(2-fluorobenzyl)amino]-2-oxoethoxy}phenyl)ethoxy]benzoic acid

HRID 898893
ノート
印刷プレビュー

反応式

HRID 898893 の反応式
[CH2:1]([N:3]([CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=1[F:34])[C:4](=[O:26])[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([CH2:13][CH2:14][O:15][C:16]2[CH:25]=[CH:24][CH:23]=[CH:22][C:17]=2[C:18]([O:20]C)=[O:19])=[CH:9][CH:8]=1)[CH3:2].O.[OH-].[Li+]>C1COCC1>[CH2:1]([N:3]([CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=1[F:34])[C:4](=[O:26])[CH2:5][O:6][C:7]1[CH:8]=[CH:9][C:10]([CH2:13][CH2:14][O:15][C:16]2[CH:25]=[CH:24][CH:23]=[CH:22][C:17]=2[C:18]([OH:20])=[O:19])=[CH:11][CH:12]=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

5

反応物 3

HCID 962WaterHCID 3939Lithium HydroxideHCID 69259940Methyl 2-[2-(4-{2-[ethyl(2-fluorobenzyl)amino]-2-oxoethoxy}phenyl)ethoxy]benzoate

生成物 1

HCID 100725002-[2-(4-{2-[Ethyl(2-fluorobenzyl)amino]-2-oxoethoxy}phenyl)ethoxy]benzoic acid収率 308.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
150 °C

実験手順

Methyl 2-[2-(4-{2-[ethyl(2-fluorobenzyl)amino]-2-oxoethoxy}phenyl)ethoxy]benzoate (0.200 g, 0.115 mmol) was dissolved in 3 ml THF in a Smith synthesiser vial and then 1.5 ml water and lithium hydroxide (0.032 g, 1.335 mmol) were added to the vial. The vial was capped and put in the microwave oven (Smith synthesiser). The reaction was then heated to 150° C. for 6 minutes. According to LC-MS the reaction was complete. The solvent was evaporated. The residue was dissolved in diethyl ether (30 ml) and washed with NaHCO3 (sat) (2×20 ml). The basic water layer was acidified to pH 1 with 2M HCl. The water layer was extracted with three portions of 20 ml of DCM which were combined, dried and evaporated to give 160 mg of pure desired product.

後処理

  1. customThe vial was capped
  2. customThe solvent was evaporated
  3. dissolutionThe residue was dissolved in diethyl ether (30 ml)
  4. washwashed with NaHCO3 (sat) (2×20 ml)
  5. extractionThe water layer was extracted with three portions of 20 ml of DCM which
  6. customdried
  7. customevaporated

出典と根拠

ORDレコード
ord-8bf9a3da95294393af7426c2540205e2
出典データセット
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07351858B2

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