Sodium Hydroxide → 4,5-Dichlorothiophene-2-carboxylic acid

HRID 844013ノート

反応式

HRID 844013 の反応式
[OH-:1].[Na+].ClCl.[Cl:5][C:6]1[CH:7]=[C:8]([C:12](=[O:14])C)[S:9][C:10]=1[Cl:11]>O.O1CCOCC1>[Cl:5][C:6]1[CH:7]=[C:8]([C:12]([OH:14])=[O:1])[S:9][C:10]=1[Cl:11]

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 24526ChlorineHCID 1488132-Acetyl-4,5-dichlorothiophene

生成物 1

HCID 3056874,5-Dichlorothiophene-2-carboxylic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 312751,4-Dioxane溶媒

反応条件

温度
50 °C

実験手順

Into a solution of sodium hydroxide (19.2 grams, 48.0 mmole) in water (30 ml) and ice (120 g) at −10° C. was bubbled Cl2 gas until 14.4 g was obtained. The solution was warmed to 50° C. and 1-(4,5-Dichloro-thiophen-2-yl)-ethanone (8.5 0 grams, 40.0 mmole) in dioxane (40 ml) was added dropwise as the temperature rose to 80-90° C. This temperature was maintained for 30 minutes. The mixture was poured into 500 ml water. This was extracted with diethyl ether, and the aqueous was treated with NaHSO3, then acidified to pH 1 with concentrated HCl. The resultant precipitate was filtered, and dried to give a white solid. (5.7 g). MW 197.04; 1H NMR (DMSO-d6) d 7.731 (1H, s).

後処理

  1. customwas obtained
  2. customrose to 80-90° C
  3. temperatureThis temperature was maintained for 30 minutes
  4. extractionThis was extracted with diethyl ether
  5. additionthe aqueous was treated with NaHSO3
  6. filtrationThe resultant precipitate was filtered
  7. customdried
  8. customto give a white solid

出典と根拠

ORDレコード
ord-2eb98e649cf0456ca3ca896981fc3a81
出典データセット
uspto-grants-2002_04
特許番号
US06380218B1

反応ノート

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