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Sodium Hydroxide → HCID 3700253、化合物

HRID 2049889
ノート
印刷プレビュー

反応式

HRID 2049889 の反応式
[Na].[H-].COCCO[Al+]OCCOC.[F:14][C:15]1[CH:30]=[CH:29][C:18]([O:19][C:20]2[CH:28]=[CH:27][CH:26]=[CH:25][C:21]=2[C:22](O)=[O:23])=[CH:17][CH:16]=1.[OH-].[Na+]>C1C=CC=CC=1>[F:14][C:15]1[CH:30]=[CH:29][C:18]([O:19][C:20]2[CH:28]=[CH:27][CH:26]=[CH:25][C:21]=2[CH2:22][OH:23])=[CH:17][CH:16]=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

5

反応物 3

HCID 14798Sodium HydroxideHCID 30083672-(4-Fluorophenoxy)benzoic acidHCID 86736934HCID 86736934、化合物

生成物 1

HCID 3700253HCID 3700253、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

反応条件

温度
0 °C

実験手順

36.1 ml of 70% sodium-bis-(2-methoxyethoxy) aluminum hydride in benzene are added dropwise over a one hour span to a stirring mixture of 15 g of 2-(4-fluorophenoxy)benzoic acid in 150 ml of benzene under nitrogen at ambient temperature. After total addition, the reaction mixture is stirred for an additional 30 minutes and then permitted to stand for 4 days. Thereafter, the reaction mixture is cooled to 0° C. before adding 100 mls of 10% sodium hydroxide while stirring. Following this addition, the layers separate and the aqueous layer is extracted twice with 100 ml portions of benzene. The combined benzene solutions are successively washed twice with 100 ml portions of water, washed once with 60 ml of saturated sodium chloride solution and dried, providing a clear yellow oil. The oil is distilled at 118.5°-121.5° C. and 0.07 mm pressure to provide the clear, colorless liquid, 2-(4-fluorophenoxy)benzyl alcohol.

後処理

  1. additionAfter total addition
  2. waitto stand for 4 days
  3. stirringwhile stirring
  4. additionthis addition
  5. customthe layers separate
  6. extractionthe aqueous layer is extracted twice with 100 ml portions of benzene
  7. washThe combined benzene solutions are successively washed twice with 100 ml portions of water
  8. washwashed once with 60 ml of saturated sodium chloride solution
  9. customdried
  10. customproviding a clear yellow oil
  11. distillationThe oil is distilled at 118.5°-121.5° C.

出典と根拠

ORDレコード
ord-d28fbc978fc94e9ab2f6ccb7ca84b64b
出典データセット
uspto-grants-1980_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04198417

反応ノート

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