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

Dimethyl Sulfoxide → 4-(tert-Butyl)-2-(1-Boc-piperidin-4-yloxy)benzaldehyde

HRID 644205
ノート
印刷プレビュー

反応式

HRID 644205 の反応式
C(Cl)(=O)C(Cl)=O.CS(C)=O.[C:11]([C:15]1[CH:22]=[CH:21][C:18]([CH2:19][OH:20])=[C:17]([O:23][CH:24]2[CH2:29][CH2:28][N:27]([C:30]([O:32][C:33]([CH3:36])([CH3:35])[CH3:34])=[O:31])[CH2:26][CH2:25]2)[CH:16]=1)([CH3:14])([CH3:13])[CH3:12].C(N(CC)CC)C>ClCCl>[C:11]([C:15]1[CH:22]=[CH:21][C:18]([CH:19]=[O:20])=[C:17]([O:23][CH:24]2[CH2:25][CH2:26][N:27]([C:30]([O:32][C:33]([CH3:36])([CH3:35])[CH3:34])=[O:31])[CH2:28][CH2:29]2)[CH:16]=1)([CH3:14])([CH3:12])[CH3:13]
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 4

HCID 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 576024554-tert-Butyl-2-(1-Boc-piperidin-4-yloxy)benzyl Alcohol

生成物 1

HCID 866342044-(tert-Butyl)-2-(1-Boc-piperidin-4-yloxy)benzaldehyde収率 101%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒
2 回

反応条件

温度
-78 °C

実験手順

To a solution of oxalyl chloride (0.30 mL, 3.46 mmol) in dichloromethane (5 mL) stirring at −78° C. under nitrogen atmosphere, dimethylsulfoxide was added dropwise (0.49 mL, 6.93 mmol). After 10 min, a solution of the crude 4-(tert-butyl)-2-(1-Boc-piperidine-4-yloxy)benzyl alcohol (0.42 g, 1.15 mmol) in dichloromethane (6 mL) was added slowly via cannula. After the addition was complete, the reaction mixture was stirred at −78° C. for 1 h. The reaction was then treated with triethylamine (1.6 mL, 11.5 mmol) and allowed to warm up to room temperature overnight. The reaction mixture was partitioned between brine and dichloromethane. The organic layer was separated and the aqueous layer was extracted with dichloromethane. The combined organic layers were dried with magnesium sulfate, filtered, and concentrated in vacuo to a brown residue which was purified on a silica gel chromatotron plate. Elution with ethyl acetate-hexanes (1:5) afforded the title compound (0.42 g, 100%) as a clear oil which foamed up under vacuum.

後処理

  1. additionAfter the addition
  2. temperatureto warm up to room temperature overnight
  3. customThe reaction mixture was partitioned between brine and dichloromethane
  4. customThe organic layer was separated
  5. extractionthe aqueous layer was extracted with dichloromethane
  6. dry with materialThe combined organic layers were dried with magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo to a brown residue which
  9. customwas purified on a silica gel chromatotron plate
  10. washElution with ethyl acetate-hexanes (1:5)

出典と根拠

ORDレコード
ord-975771b404524465ad2dc41601721cb1
出典データセット
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07700628B2

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