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Potassium Hydroxide → 1-Hydroxymethyl-7-Methoxynaphthalene

HRID 1370767
ノート
印刷プレビュー

反応式

HRID 1370767 の反応式
C([O:4][CH2:5][C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([O:16][CH3:17])[CH:14]=2)[CH:9]=[CH:8][CH:7]=1)(=O)C.[OH-].[K+]>CO.O>[CH3:17][O:16][C:13]1[CH:14]=[C:15]2[C:10]([CH:9]=[CH:8][CH:7]=[C:6]2[CH2:5][OH:4])=[CH:11][CH:12]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 14797Potassium HydroxideHCID 185132061-Acetoxymethyl-7-methoxynaphthalene

生成物 1

HCID 154530791-Hydroxymethyl-7-Methoxynaphthalene

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

34.5 g (0.15 mol) of the compound obtained in Step A are dissolved in 300 ml of methanol. 35 g (4 eq) of potassium hydroxide dissolved in 35 ml of water are added with vigorous stirring. After 3 hours at room temperature, the reaction mixture is hydrolysed over a mixture of ice/concentrated hydrochloric acid. The creamy white precipitate which forms is filtered off, washed several times with ice-cold water and dried over P2O5 using a dessicator. The title alcohol is recrystallised from a mixture of CH2Cl2/cyclohexane to yield white needles.

後処理

  1. additionare added with vigorous stirring
  2. additionthe reaction mixture is hydrolysed over a mixture of ice/concentrated hydrochloric acid
  3. filtrationThe creamy white precipitate which forms is filtered off
  4. washwashed several times with ice-cold water
  5. dry with materialdried over P2O5 using a dessicator
  6. customThe title alcohol is recrystallised from a mixture of CH2Cl2/cyclohexane
  7. customto yield white needles

出典と根拠

ORDレコード
ord-029cb000bdc8442e92e5896d1e60f42d
出典データセット
uspto-grants-2003_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06583319B1

反応ノート

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