Sodium Carbonate → Phloroglucinol

HRID 1763413ノート

反応式

HRID 1763413 の反応式
C([O:3][C:4]1[CH:11]=[C:9]([OH:10])[CH:8]=[C:6]([OH:7])[CH:5]=1)C.C(=O)([O-])[O-].[Na+].[Na+]>Cl>[C:4]1([CH:11]=[C:9]([OH:10])[CH:8]=[C:6]([OH:7])[CH:5]=1)[OH:3]

参加物

4

反応物 2

HCID 10340Sodium CarbonateHCID 1199281,3-Benzenediol, 5-ethoxy-

生成物 1

HCID 359Phloroglucinol収率 86%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

2 g of phloroglucinol monoethyl ether are stirred in 100 ml of concentrated hydrochloric acid (35%) at room temperature for 2 days. The mixture is then partially neutralised (pH 2-3) with aqueous sodium carbonate solution, the precipitated sodium chloride is filtered off and the filtrate is extracted with 150 ml of ether in a Kutscher-Steudel extractor for 18 hours. The ether extract is dried over sodium sulphate and concentrated, there being obtained 1.4 g to 1.55 g (86% to 95%) of phloroglucinol which has a melting point of 209°-210° C. after recrystallisation from water.

後処理

  1. filtrationthe precipitated sodium chloride is filtered off
  2. extractionthe filtrate is extracted with 150 ml of ether in a Kutscher-Steudel extractor for 18 hours
  3. extractionThe ether extract
  4. dry with materialis dried over sodium sulphate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-a2847c2953fa44bca86695e4da772b01
出典データセット
uspto-grants-1978_09
特許番号
US04112003

反応ノート

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