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Hydrochloric Acid → (4-Carboxymethoxyphenyl)-4-methoxyphenylcarbinol

HRID 1649955
ノート
印刷プレビュー

反応式

HRID 1649955 の反応式
[CH3:1][O:2][C:3]1[CH:21]=[CH:20][C:6]([C:7]([C:9]2[CH:19]=[CH:18][C:12]([O:13][CH2:14][C:15]([OH:17])=[O:16])=[CH:11][CH:10]=2)=[O:8])=[CH:5][CH:4]=1.[BH4-].[Na+].Cl>CO.CN1CCOCC1>[C:15]([CH2:14][O:13][C:12]1[CH:11]=[CH:10][C:9]([CH:7]([C:6]2[CH:20]=[CH:21][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)[OH:8])=[CH:19][CH:18]=1)([OH:17])=[O:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 4311764Sodium borohydrideHCID 143045424-(4-Methoxybenzoyl)phenoxyacetic acid

生成物 1

HCID 13966820(4-Carboxymethoxyphenyl)-4-methoxyphenylcarbinol

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 79724-Methylmorpholine溶媒

実験手順

11.2 g of 4-(4-methoxybenzoyl)phenoxyacetic acid are dissolved in 600 ml of 80% strength methanol (reflux), and 4.4 ml of N-methylmorpholine are added. 6 g of sodium borohydride are added in portions over the course of two hours, and the reaction is continued under reflux conditions for 3 hours. The mixture is cooled to room temperature and acidified to pH 2.5 with 3N HCl. The methanol is distilled off, the aqueous phase is extracted with ethyl acetate, and the organic phase is washed with brine and dried over sodium sulfate. After removal of the ethyl acetate by distillation there remains a white amorphous powder. The product is used directly for the next reaction.

後処理

  1. additionare added
  2. distillationThe methanol is distilled off
  3. extractionthe aqueous phase is extracted with ethyl acetate
  4. washthe organic phase is washed with brine
  5. dry with materialdried over sodium sulfate
  6. customAfter removal of the ethyl acetate
  7. distillationby distillation
  8. customThe product is used directly for the next reaction

出典と根拠

ORDレコード
ord-8bed4e1881904129ba0bbf6e1c56e831
出典データセット
uspto-grants-1990_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04922015

反応ノート

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