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 → HCID 9908951、化合物

HRID 275969
ノート
印刷プレビュー

反応式

HRID 275969 の反応式
[OH-].[Li+].[CH2:3]([O:5][CH:6]([CH2:12][C:13]1[CH:18]=[CH:17][C:16]([O:19][CH2:20][CH:21]=[C:22]2[C:34]3[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=3[C:28]3[C:23]2=[CH:24][CH:25]=[CH:26][CH:27]=3)=[CH:15][CH:14]=1)[C:7]([O:9]CC)=[O:8])[CH3:4]>C(O)C>[CH2:3]([O:5][CH:6]([CH2:12][C:13]1[CH:18]=[CH:17][C:16]([O:19][CH2:20][CH:21]=[C:22]2[C:34]3[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=3[C:28]3[C:23]2=[CH:24][CH:25]=[CH:26][CH:27]=3)=[CH:15][CH:14]=1)[C:7]([OH:9])=[O:8])[CH3:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 9823905HCID 9823905、化合物

生成物 1

HCID 9908951HCID 9908951、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Lithium hydroxide (1M, 1.0 ml, 1.0 mmol) was added to a suspension of ethyl 2-ethoxy-3-[4-(2-fluoren-9-ylidene-ethoxy)-phenyl]-propionate (0.214 g, 0.5 mmol) in ethanol (5 ml) and the resulting mixture heated to gentle reflux for 30 min. The cooled mixture was partitioned between water (30 ml) and dichloromethane (20 ml), acidified to pH 1 by adding 1N hydrochloric acid (3 ml), and the organic phase collected. The aqueous phase was further extracted with dichloromethane (3×20 ml) and the combined organics were washed with brine, dried (MgSO4) and evaporated to give a yellow gum. The product was purified by column chromatography on silica gel (3% methanol in dichloromethane eluent) to give 2-ethoxy-3-[4-(2-fluoren-9-ylidene-ethoxy)-phenyl]-propionic acid, as a yellow solid; 0.104 g (51%).

後処理

  1. temperaturethe resulting mixture heated
  2. temperatureto gentle reflux for 30 min
  3. customThe cooled mixture was partitioned between water (30 ml) and dichloromethane (20 ml)
  4. additionby adding 1N hydrochloric acid (3 ml)
  5. customthe organic phase collected
  6. extractionThe aqueous phase was further extracted with dichloromethane (3×20 ml)
  7. washthe combined organics were washed with brine
  8. dry with materialdried (MgSO4)
  9. customevaporated
  10. customto give a yellow gum
  11. customThe product was purified by column chromatography on silica gel (3% methanol in dichloromethane eluent)

出典と根拠

ORDレコード
ord-d84edb0a33ed4b9ca063fa142a2854db
出典データセット
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06353018B1

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