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

Formic Acid → HCID 19784640、化合物

HRID 257154
ノート
印刷プレビュー

反応式

HRID 257154 の反応式
[CH:1]1([CH2:7][CH:8]2[CH:13]([OH:14])[CH2:12][C:11]([CH3:16])([CH3:15])[NH:10][C:9]2([CH3:18])[CH3:17])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH:19](O)=O.C=O.[OH-].[Na+]>O1CCOCC1>[CH:1]1([CH2:7][CH:8]2[CH:13]([OH:14])[CH2:12][C:11]([CH3:16])([CH3:15])[N:10]([CH3:19])[C:9]2([CH3:18])[CH3:17])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1
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 284Formic AcidHCID 712FormaldehydeHCID 14798Sodium HydroxideHCID 19784639HCID 19784639、化合物

生成物 1

HCID 19784640HCID 19784640、化合物収率 98.5%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

反応条件

温度
80 °C

実験手順

Into a 100 ml-flask equipped with a thermometer, a cooling tube, a dropping funnel and a magnetic stirrer were introduced 3.8 g (15 mmol) of 3-cyclohexylmethyl-2,2,6,6-tetramethyl-4-piperidinol prepared in Example B1, 70 ml of dioxane and 0.78 g (17 mmol) of formic acid, and the content of the flask was heated to 80° C. When the temperature of the content of the flask was constant, 2.44 g (30 mmol) of 37% aqueous formaldehyde dissolved in 20 ml of dioxane was added gradually through the dropping funnel, followed by heating at the temperature for 10 hours. The content of the flask was cooled to room temperature, and 5% aqueous NaOH was added so that the pH became 8, followed by extraction with 200 ml of diethylether. The extract obtained was washed with 30 ml of water 3 times, 10 g of magnesium sulfate was added and, after it was kept standing for ca. 2 hours, the solution was filtered and concentrated to give 3.95 g (yield: 98%) of the title compound as a white solid product.

後処理

  1. customInto a 100 ml-flask equipped with a thermometer, a cooling tube, a dropping funnel and a magnetic stirrer
  2. additionwas added gradually through the dropping funnel
  3. temperatureby heating at the temperature for 10 hours
  4. temperatureThe content of the flask was cooled to room temperature
  5. extractionfollowed by extraction with 200 ml of diethylether
  6. customThe extract obtained
  7. washwas washed with 30 ml of water 3 times, 10 g of magnesium sulfate
  8. additionwas added
  9. filtrationthe solution was filtered
  10. concentrationconcentrated

出典と根拠

ORDレコード
ord-a58843332b3b4da5b05082d89b70e4b5
出典データセット
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05260443

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