Water → 4-Aminomethylbenzyl 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl ether

HRID 1599117

反応式

HRID 1599117 の反応式
[CH3:1][C:2]1([CH3:24])[CH2:11][CH2:10][C:9]([CH3:13])([CH3:12])[C:8]2[CH:7]=[C:6]([O:14][CH2:15][C:16]3[CH:21]=[CH:20][C:19]([C:22]#[N:23])=[CH:18][CH:17]=3)[CH:5]=[CH:4][C:3]1=2.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.S([O-])([O-])(=O)=O.[Na+].[Na+]>CCOCC>[CH3:1][C:2]1([CH3:24])[CH2:11][CH2:10][C:9]([CH3:12])([CH3:13])[C:8]2[CH:7]=[C:6]([O:14][CH2:15][C:16]3[CH:21]=[CH:20][C:19]([CH2:22][NH2:23])=[CH:18][CH:17]=3)[CH:5]=[CH:4][C:3]1=2

参加物

6

反応物 4

HCID 962WaterHCID 24436Sodium SulfateHCID 148505774-Cyanobenzyl 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl etherHCID 21226445Aluminium lithium hydride

生成物 1

HCID 148505814-Aminomethylbenzyl 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl ether

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

A suspension of 3 g (9.4 mmol) of 4-cyanobenzyl 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl ether in 60 ml of ether was added dropwise under nitrogen to a suspension of I g (26 mmol) of lithium aluminum hydride in 50 ml of dry ether at 25° C. The mixture was then stirred under reflux for 3 h, cooled and hydrolyzed cautiously with water and sodium sulfate solution. The mixture was extracted three times with ether, and the combined ether extracts were washed with water, dried over Na2SO4 and concentrated. 3 g of the title compound of melting point 77°-79° C. remained.

後処理

  1. additionwas added dropwise under nitrogen to a suspension of I
  2. customat 25° C
  3. temperatureunder reflux for 3 h
  4. temperaturecooled
  5. extractionThe mixture was extracted three times with ether
  6. washthe combined ether extracts were washed with water
  7. dry with materialdried over Na2SO4
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-fbe3f53d8e1c49b6bbce028fc00e86b4
出典データセット
uspto-grants-1998_04
特許番号
US05739374

関連ノート

読み込み中…