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

Acetaldehyde → Ethyl 2-(6-tert-butoxycarbonylamino-pyridin-3-ylmethyl)-but-2-enoic acid ethyl ester

HRID 1789872
ノート
印刷プレビュー

反応式

HRID 1789872 の反応式
[H-].[Na+].[CH2:3]([O:5][C:6](=[O:31])[CH:7](P(OCC)(OCC)=O)[CH2:8][C:9]1[CH:10]=[N:11][C:12]([NH:15][C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])=[CH:13][CH:14]=1)[CH3:4].C(=O)C.[CH2:35]1[CH2:39]O[CH2:37][CH2:36]1>>[CH2:3]([O:5][C:6](=[O:31])[C:7]([CH2:8][C:9]1[CH:10]=[N:11][C:12]([NH:15][C:16]([O:18][C:19]([CH3:20])([CH3:21])[CH3:22])=[O:17])=[CH:13][CH:14]=1)=[C:35]([CH2:36][CH3:37])[CH3:39])[CH3:4]
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 4

HCID 177Acetaldehyde2 回HCID 8028Tetrahydrofuran2 回HCID 24758Sodium hydrideHCID 220360143-(6-Tert-butoxycarbonylamino-pyridin-3-yl)-2-(diethoxyphosphoryl)-propionic acid ethyl ester

生成物 1

HCID 57028003Ethyl 2-(6-tert-butoxycarbonylamino-pyridin-3-ylmethyl)-but-2-enoic acid ethyl ester

反応条件

温度
0 °C

実験手順

To a suspension of NaH (278.8 mg, 60% in mineral oil, 6.97 mmol) in THF (25 mL) at 0° C. was added a solution of 3-(6-tert-butoxycarbonylamino-pyridin-3-yl)-2-(diethoxyphosphoryl)-propionic acid ethyl ester (2.5 g, 5.81 mmol) in THF (30 mL). The reaction mixture was allowed to stir at 0° C. for 1 h. To the reaction was added acetaldehyde (512 mg, 11.6 mmol) dropwise at 0° C. The reaction mixture was allowed to warm to room temperature and then stir for 16 h. Acetaldehyde (2.0 g) was added to the reaction vessel and the reaction mixture was allowed to stir at room temperature for an additional 16 h. The reaction was quenched with the slow addition of saturated aqueous ammonium chloride (30 mL). The mixture was extracted with EtOAc, washed with brine and dried to afford the crude product. The crude product was purified by column chromatography (EtOAc/hexane, 1:8) to give ethyl 2-(6-tert-butoxycarbonylamino-pyridin-3-ylmethyl)-but-2-enoic acid ethyl ester as a mixture of isomers (1.1 g, 60%).

後処理

  1. temperatureto warm to room temperature
  2. stirringstir for 16 h
  3. stirringto stir at room temperature for an additional 16 h
  4. customThe reaction was quenched with the slow addition of saturated aqueous ammonium chloride (30 mL)
  5. extractionThe mixture was extracted with EtOAc
  6. washwashed with brine
  7. customdried
  8. customto afford the crude product
  9. customThe crude product was purified by column chromatography (EtOAc/hexane, 1:8)

出典と根拠

ORDレコード
ord-fb4ce0cb2e1f4a64b1bdf58712ab1ba0
出典データセット
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07071175B1

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