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Sulfuric Acid → HCID 178513810、化合物

HRID 76373
ノート
印刷プレビュー

反応式

HRID 76373 の反応式
S(=O)(=O)(O)O.[F:6][C:7]1[N:12]=[C:11]([C:13]#[N:14])[C:10]([OH:15])=[N:9][CH:8]=1.[OH-:16].[Na+]>O>[F:6][C:7]1[N:12]=[C:11]([C:13]([NH2:14])=[O:16])[C:10]([OH:15])=[N:9][CH:8]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 178510584HCID 178510584、化合物

生成物 1

HCID 178513810HCID 178513810、化合物収率 92.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

14.39 g of concentrated sulfuric acid was added to 3.45 g of the oily 6-fluoro-3-hydroxypyrazine-2-carbonitrile, and the resulting mixture was stirred at 50° C. for 4 hours. The reaction mixture was then added dropwise over a period of 20 minutes to 44.5 ml of water that had been cooled to 3° C. Following completion of the dropwise addition, the resulting mixture was stirred for 20 minutes at a temperature of not more than 10° C. Subsequently, 10.17 g of a 28% aqueous solution of sodium hydroxide was added dropwise to the reaction mixture over a period of 15 minutes. Following completion of the dropwise addition, the mixture was stirred at the same temperature for 30 minutes. The solid product was then filtered off, and washed with 18 ml of water, yielding 2.22 g (yield: 92.3%) of 6-fluoro-3-hydroxypyrazine-2-carboxamide.

後処理

  1. temperaturehad been cooled to 3° C
  2. additioncompletion of the dropwise addition
  3. stirringthe resulting mixture was stirred for 20 minutes at a temperature of not more than 10° C
  4. additioncompletion of the dropwise addition
  5. stirringthe mixture was stirred at the same temperature for 30 minutes
  6. filtrationThe solid product was then filtered off
  7. washwashed with 18 ml of water

出典と根拠

ORDレコード
ord-0c2eb05f05ba43aab6ad0f97b9786b37
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08835636B2

反応ノート

読み込み中…

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