Aluminium lithium hydride → 2,2-Bis-(2,2,2-trifluoro-ethyl)-propane-1,3-diamine

HRID 1024371

반응식

HRID 1024371 반응식
[H-].[H-].[H-].[H-].[Li+].[Al+3].[F:7][C:8]([F:21])([F:20])[CH2:9][C:10]([CH2:15][C:16]([F:19])([F:18])[F:17])([C:13]#[N:14])[C:11]#[N:12]>CCOCC>[F:7][C:8]([F:20])([F:21])[CH2:9][C:10]([CH2:15][C:16]([F:17])([F:18])[F:19])([CH2:11][NH2:12])[CH2:13][NH2:14]

참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 866254102,2-Bis-(2,2,2-trifluoro-ethyl)-malononitrile

생성물 1

HCID 866254112,2-Bis-(2,2,2-trifluoro-ethyl)-propane-1,3-diamine수율 91.5%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

340 mg LiAlH4 (8.95 mmol) was suspended in 15 ml dry Et2O and cooled in an ice bath. A solution of 760 mg 2,2-Bis-(2,2,2-trifluoro-ethyl)-malononitrile in Et2O was added dropwise at such a rate that the temperature was kept below 20° C. The mixture was stirred overnight at room temperature, cooled in an ice bath, and quenched by adding H2O (0.35 ml), 2M aqueous NaOH (0.70 ml), and again H2O (0.35 ml). The suspension was filtered, the filtercake was washed with Et2O, and the combined filtrates were evaporated to dryness under reduced pressure to give 0.72 g of an oil. This material was used in the subsequent step without further purification.

후처리

  1. temperaturecooled in an ice bath
  2. customwas kept below 20° C
  3. temperaturecooled in an ice bath
  4. customquenched
  5. additionby adding H2O (0.35 ml), 2M aqueous NaOH (0.70 ml), and again H2O (0.35 ml)
  6. filtrationThe suspension was filtered
  7. washthe filtercake was washed with Et2O
  8. customthe combined filtrates were evaporated to dryness under reduced pressure

출처 및 근거

ORD 기록
ord-64914aac893b45258fadccef246221ed
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722887B2

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