Tetrahydrofuran → HCID 178436223、化合物

HRID 254462

反応式

HRID 254462 の反応式
CO[C:3]1[CH:8]=[CH:7][CH:6]=[C:5](OC)[C:4]=1/[CH:11]=[N:12]/[CH:13]([CH:17]([CH3:19])[CH3:18])[CH:14]([CH3:16])[CH3:15].[CH2:20]([Li])[CH3:21].[CH2:23]1COC[CH2:24]1>C1CCCCC1.C1C=CC=CC=1>[CH2:23]([C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH2:20][CH3:21])[C:4]=1/[CH:11]=[N:12]/[CH:13]([CH:17]([CH3:19])[CH3:18])[CH:14]([CH3:16])[CH3:15])[CH3:24]

参加物

5

反応物 3

HCID 8028TetrahydrofuranHCID 178491344HCID 178491344、化合物HCID 178506846HCID 178506846、化合物

生成物 1

HCID 178436223HCID 178436223、化合物

試薬・触媒・溶媒 1

HCID 18624872Benzene--cyclohexane (1/1)溶媒

反応条件

温度
-20 °C

実験手順

To a solution of 16.0 g (61 mmol) [1-(2,6-dimethoxy-phenyl)-meth-(E)-ylidene]-(1-isopropyl-2-methyl-propyl)-amine in 80 ml dry THF cooled to −40° C. were added 364 ml of a 0.5M solution of ethyl lithium in cyclohexane/benzene drop-wise to keep temperature below −20° C. Then the mixture was stirred at −20° C. for further 30 min and the reaction quenched by addition of water. The aqueous phase was extracted with ethyl acetate, the combined extracts washed with brine, dried over Na2SO4, filtered and evaporated: 15.6 g (E)-[1-(2,6-diethyl-phenyl)-methylidene]-(1-isopropyl-2-methyl-propyl)-amine as colourless liquid: MS (EI): 259.2 (M+.), 216.3 ((M-(CH3)2CH)+.)), 160.1 (((M-(((CH3)2CH)2CH))+.), 100%).

後処理

  1. customtemperature below −20° C
  2. customthe reaction quenched by addition of water
  3. extractionThe aqueous phase was extracted with ethyl acetate
  4. washthe combined extracts washed with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. customevaporated

出典と根拠

ORDレコード
ord-dc4bb5f122174db290298dd15ddb2ef0
出典データセット
uspto-grants-2011_01
特許番号
US07875645B2

関連ノート

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