Sulfuric Acid → HCID 19365521、化合物

HRID 849964ノート

反応式

HRID 849964 の反応式
S(=O)(=O)(O)O.[NH2:6][CH:7]([C:10]1[CH:15]=[CH:14][C:13]([F:16])=[CH:12][C:11]=1[F:17])[C:8]#[N:9].[OH2:18].N>O>[NH2:6][CH:7]([C:10]1[CH:15]=[CH:14][C:13]([F:16])=[CH:12][C:11]=1[F:17])[C:8]([NH2:9])=[O:18]

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 12896473Azane;hydrateHCID 167677482-Amino-2-(2,4-difluorophenyl)acetonitrile

生成物 1

HCID 19365521HCID 19365521、化合物収率 61%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Then, 51 g of concentrated sulfuric acid was added to 2.67 g of water, to which 40 g of 2-amino-2-(2,4-difluorophenyl)acetonitrile was added under ice cooling, and the mixture was heated at 50° to 60° C. under stirring for 3 hours. After completion of the reaction, the reaction mixture was poured into 250 ml of concentrated ammonia water cooled with ice in such a manner that the temperature of the solution became not higher than 20° C. The precipitated crystals were collected by filtration, and the filtrate was extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated. The residue was combined with the previously collected crystals, followed by recrystallization, which afforded 27.2 g (yield, 61%) of 2-amino-2-(2,4-difluorophenyl)acetamide, m.p. 142.9° C.

後処理

  1. additionwas added under ice cooling
  2. temperaturethe mixture was heated at 50° to 60° C.
  3. customAfter completion of the reaction
  4. temperaturecooled with ice in such a manner that the temperature of the solution
  5. custombecame not higher than 20° C
  6. filtrationThe precipitated crystals were collected by filtration
  7. extractionthe filtrate was extracted with ethyl acetate
  8. washThe organic layer was washed with saturated sodium chloride solution
  9. dry with materialdried with anhydrous magnesium sulfate
  10. concentrationconcentrated
  11. customfollowed by recrystallization, which

出典と根拠

ORDレコード
ord-04bb564b7b0c460daeaec552d5569e2a
出典データセット
uspto-grants-2000_01
特許番号
US06015774

反応ノート

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