Hydrochloric Acid → 1-(3-Chloro-2,4-dihydroxy-phenyl)ethanone

HRID 1161021

反応式

HRID 1161021 の反応式
[CH3:1][C:2]([C:4]1[CH:5]=[CH:6][C:7]([OH:11])=[CH:8][C:9]=1[OH:10])=[O:3].[OH-].[Na+].[Cl:14][O-].[Na+].Cl>O>[Cl:14][C:8]1[C:9]([OH:10])=[C:4]([C:2](=[O:3])[CH3:1])[CH:5]=[CH:6][C:7]=1[OH:11]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 69902',4'-DihydroxyacetophenoneHCID 14798Sodium HydroxideHCID 23665760Sodium Hypochlorite

生成物 1

HCID 574382941-(3-Chloro-2,4-dihydroxy-phenyl)ethanone収率 65%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 2,4-dihydroxyacetophenone (6 g, 39.4 mmol), aqueous 1M sodium hydroxide (41.4 mL, 41.4 mmol) and water (200 mL) is stirred at room temperature. An aqueous 1.6M solution of sodium hypochlorite (32 mL) is added over a 1 hr period. The resulting dark brown solution is stirred 18 hr at room temperature. The reaction mixture is adjusted to a pH of 2-3 with concentrated aqueous hydrochloric acid. The resulting suspension is filtered and washed with water (4×100 mL). The filtered solid was dried under vacuum at 45° C. for 2.5 days to give the title compound (4.8 g, 65%) as a brown solid. LCMS 1 187 M+.

後処理

  1. filtrationThe resulting suspension is filtered
  2. washwashed with water (4×100 mL)
  3. customThe filtered solid was dried under vacuum at 45° C. for 2.5 days

出典と根拠

ORDレコード
ord-c6985bac739c4f40be1b9f741ad7ff3b
出典データセット
uspto-grants-2010_10
特許番号
US07816523B2

関連ノート

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