Sodium Chloride → HCID 15908685、化合物

HRID 271656

反応式

HRID 271656 の反応式
Cl[O-].[Na+].[OH:4][C:5]1[C:14]([CH3:15])=[CH:13][CH:12]=[CH:11][C:6]=1[C:7]([O:9]C)=[O:8].[Na+].[I-:17].[OH-].[Na+].[Na+].[Cl-]>CO.O.C(Cl)Cl>[OH:4][C:5]1[C:14]([CH3:15])=[CH:13][C:12]([I:17])=[CH:11][C:6]=1[C:7]([OH:9])=[O:8]

参加物

9

反応物 5

HCID 5234Sodium ChlorideHCID 5238Sodium IodideHCID 14798Sodium HydroxideHCID 31835Benzoic acid, 2-hydroxy-3-methyl-, methyl esterHCID 23665760Sodium Hypochlorite

生成物 1

HCID 15908685HCID 15908685、化合物

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
-5 °C

実験手順

14.9 mL (24.1 mmol) sodium hypochlorite solution (10 percent by weight in water) is added dropwise to a solution of 4.0 g (24.1 mmol) methyl 2-hydroxy-3-methyl-benzoate, 3.6 g (24.1 mmol) NaI, 0.96 g (24.1 mmol) NaOH in 100 mL MeOH at −5° C. over 40 min. The reaction is stirred for 30 min at −5° C. and 5 days at RT. The solvent is eliminated i.vac. and the residue is taken up in 80 mL water and 50 mL DCM. After the organic phase has been saturated with NaCl it is extracted twice with DCM. The combined organic extracts are filtered and the solvent is eliminated i.vac. The product is further reacted without any more purification.

後処理

  1. extractionis extracted twice with DCM
  2. filtrationThe combined organic extracts are filtered
  3. customThe product is further reacted without any more purification

出典と根拠

ORDレコード
ord-b5bebfbd22c54301ab2733631abb790c
出典データセット
uspto-grants-2008_11
特許番号
US07452911B2

関連ノート

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