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

HRID 844013노트

반응식

HRID 844013 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 3056874,5-Dichlorothiophene-2-carboxylic acid

시약·촉매·용매 2

HCID 962Water용매2회HCID 312751,4-Dioxane용매

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온도
50 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-2eb98e649cf0456ca3ca896981fc3a81
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06380218B1

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