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N-[4-(1H-Imidazol-1-yl)butyl]formamide → 4-(1H-Imidazol-1-yl)-N-methylbutan-1-amine

HRID 1583428
ノート
印刷プレビュー

反応式

HRID 1583428 の反応式
[N:1]1([CH2:6][CH2:7][CH2:8][CH2:9][NH:10][CH:11]=O)[CH:5]=[CH:4][N:3]=[CH:2]1>O1CCCC1>[N:1]1([CH2:6][CH2:7][CH2:8][CH2:9][NH:10][CH3:11])[CH:5]=[CH:4][N:3]=[CH:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 13557541N-[4-(1H-Imidazol-1-yl)butyl]formamide

生成物 1

HCID 135575404-(1H-Imidazol-1-yl)-N-methylbutan-1-amine収率 68%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 58.8 g of N-[4-(1H-imidazol-1-yl)butyl]formamide in 480 ml of dry tetrahydrofuran was treated with 87.0 ml of 10 Molar borane methyl sulfide complex in tetrahydrofuran. The reaction mixture was heated to reflux for 18 hours under an argon atmosphere, cooled in an ice bath and quenched with 400 ml of methanol. The solvent was removed, the methanol addition and evaporation repeated, and the residue was made acidic with hydrochloric acid and was stirred over night. The mixture was made basic with sodium hydroxide solution and was extracted with dichloromethane. The combined organic layers were dried over potassium carbonate and evaporated to give an oil which was distilled to give 35.9 g (68%) of 4-(1H-imidazol-1-yl)-N-methylbutanamine, bp 130°-135° C./0.3 mm. The product was further characterized as the picrate, mp 111-113.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 18 hours under an argon atmosphere
  3. temperaturecooled in an ice bath
  4. customquenched with 400 ml of methanol
  5. customThe solvent was removed
  6. additionthe methanol addition and evaporation
  7. extractionwas extracted with dichloromethane
  8. dry with materialThe combined organic layers were dried over potassium carbonate
  9. customevaporated
  10. customto give an oil which
  11. distillationwas distilled

出典と根拠

ORDレコード
ord-4403d35c0e074fb4896d16a2efb5da5e
出典データセット
uspto-grants-1985_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04551460

反応ノート

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