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

Piperidine → HCID 58981682、化合物

HRID 1816364
ノート
印刷プレビュー

反応式

HRID 1816364 の反応式
[CH:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]#[C:10][CH2:11][CH2:12][O:13][S:14]([C:17]2[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][CH:18]=2)(=[O:16])=[O:15])=[CH:5][CH:4]=1)=O.[NH:24]1[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[OH-].[Na+]>C(Cl)Cl.C(O)(=O)C>[N:24]1([CH2:1][C:3]2[CH:8]=[CH:7][C:6]([C:9]#[C:10][CH2:11][CH2:12][O:13][S:14]([C:17]3[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][CH:18]=3)(=[O:16])=[O:15])=[CH:5][CH:4]=2)[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8082PiperidineHCID 14798Sodium HydroxideHCID 5049666Sodium triacetoxyborohydrideHCID 44243538HCID 44243538、化合物

生成物 1

HCID 58981682HCID 58981682、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒
HCID 6344
Dichloromethane
溶媒

実験手順

A solution of the product of Example 8 (2.0 g), piperidine (0.91 mL), and acetic acid (0.42 mL) in DCM (100 mL) was treated with sodium triacetoxyborohydride (1.95 g) at room temperature. After 16 h, the resulting mixture was treated with 10% aqueous sodium hydroxide (30 mL). The aqueous phase was extracted with DCM (2×300 mL). The combined organic phases were dried (magnesium sulfate) and concentrated under reduced pressure. The residue was diluted in DCM (100 mL) and passed through a pad of silica gel. The pad was washed with DCM (3×200 mL). The combined filtrate was concentrated under reduced pressure, giving the title compound as a brown oil (2.3 g).

後処理

  1. extractionThe aqueous phase was extracted with DCM (2×300 mL)
  2. dry with materialThe combined organic phases were dried (magnesium sulfate)
  3. concentrationconcentrated under reduced pressure
  4. additionThe residue was diluted in DCM (100 mL)
  5. washThe pad was washed with DCM (3×200 mL)
  6. concentrationThe combined filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-50ec347554b848b2b1c910a6bc2bc8a1
出典データセット
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06884803B2

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