Sodium hydride → 2,2,2-Trifluoro-N-(hex-5-EN-1-YL)-N-methylacetamide

HRID 1516666

反応式

HRID 1516666 の反応式
[H-].[Na+].[CH3:3][NH:4][C:5](=[O:10])[C:6]([F:9])([F:8])[F:7].Br[CH:12]=[CH:13][CH2:14][CH2:15][CH2:16][CH3:17]>CN(C=O)C>[CH2:17]([N:4]([CH3:3])[C:5](=[O:10])[C:6]([F:9])([F:8])[F:7])[CH2:16][CH2:15][CH2:14][CH:13]=[CH2:12]

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 69948Acetamide, 2,2,2-trifluoro-N-methyl-HCID 2873381-Bromo-1-hexene

生成物 1

HCID 575787592,2,2-Trifluoro-N-(hex-5-EN-1-YL)-N-methylacetamide収率 85%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

Sodium hydride (1.05 eq) was slowly added at 0° C. to a solution of N-methyltrifluoro-acetamide (25 g) in DMF (140 mL). The mixture was stirred for 1 h at room temperature under nitrogen. Then, a solution of bromohexene (32.1 g) in DMF (25 mL) was added dropwise and the mixture was heated to 70° C. for 12 hours. The reaction mixture was poured on water (200 mL) and extracted with ether (4×50 mL), dried (MgSO4), filtered and evaporated to give 35 g of the target product 18 as a yellowish oil which was used without further purification in the next step.

後処理

  1. temperaturethe mixture was heated to 70° C. for 12 hours
  2. additionThe reaction mixture was poured on water (200 mL)
  3. extractionextracted with ether (4×50 mL)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customevaporated

出典と根拠

ORDレコード
ord-5b7514c79ad1442eb38e6d92b9a1e338
出典データセット
uspto-grants-2012_07
特許番号
US08227407B2

関連ノート

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