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HCID 12789562、化合物 → 4-(2'-Hydroxymethylphenoxy)benzyl alcohol

HRID 1732725
ノート
印刷プレビュー

反応式

HRID 1732725 の反応式
C([O:3][C:4]([C:6]1[CH:21]=[CH:20][C:9]([O:10][C:11]2[CH:19]=[CH:18][CH:17]=[CH:16][C:12]=2[C:13](O)=[O:14])=[CH:8][CH:7]=1)=O)C.[H-].[Al+3].[Li+].[H-].[H-].[H-]>O1CCCC1>[OH:14][CH2:13][C:12]1[CH:16]=[CH:17][CH:18]=[CH:19][C:11]=1[O:10][C:9]1[CH:20]=[CH:21][C:6]([CH2:4][OH:3])=[CH:7][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 12789562HCID 12789562、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 538895684-(2'-Hydroxymethylphenoxy)benzyl alcohol収率 88.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 2-(4'-ethoxycarbonylphenoxy)benzoic acid (35 g) in dry tetrahydrofuran (120 ml) was added dropwise to a stirred suspension of lithium aluminum hydride (9.3 g) in dry tetrahydrofuran (300 ml) at room temperature. After the addition, the mixture was refluxed with stirring for 4 hours, and then the excess of lithium aluminum hydride was destroyed by cautious addition of water. The mixture was concentrated and dilute hydrochloric acid was added to the residue. The resulting mixture was extracted with chloroform and the extracts were washed with water. Concentration of the dried extracts gave crude 4-(2'-hydroxymethylphenoxy)benzyl alcohol (25 g) as an oil, IRνmaxfilm cm-1 : 3300 (OH).

後処理

  1. additionAfter the addition
  2. temperaturethe mixture was refluxed
  3. customthe excess of lithium aluminum hydride was destroyed by cautious addition of water
  4. concentrationThe mixture was concentrated
  5. additiondilute hydrochloric acid was added to the residue
  6. extractionThe resulting mixture was extracted with chloroform
  7. washthe extracts were washed with water

出典と根拠

ORDレコード
ord-9dbb2cd23ff84dbc94aca82a4555a30d
出典データセット
uspto-grants-1980_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04238620

反応ノート

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