Tert-Butylamine → HCID 14795576、化合物

HRID 1084784

反応式

HRID 1084784 の反応式
[Li].[N:2]([N:4]([C:12]([CH3:15])([CH3:14])[CH3:13])[CH:5]1[CH2:10][CH2:9][CH2:8][CH2:7][CH:6]1[OH:11])=O.O1C2CCCCC12.C(N)(C)(C)C.N([O-])=O.[Na+].[ClH:32]>>[ClH:32].[C:12]([N:4]([CH:5]1[CH2:10][CH2:9][CH2:8][CH2:7][CH:6]1[OH:11])[NH2:2])([CH3:15])([CH3:13])[CH3:14]

参加物

6

反応物 5

HCID 6385Tert-ButylamineHCID 9246Cyclohexene oxideHCID 3028194LithiumHCID 21652828HCID 21652828、化合物HCID 86602196Hydrochloride sodium nitrite

生成物 1

HCID 14795576HCID 14795576、化合物

反応条件

温度
50 °C

実験手順

10 g of lithium alanate are added in portions of 1 g to a solution of 38.8 g of N-nitroso-tert.-butyl-(2-hydroxycyclohexyl)amine (obtained by heating 1,2-epoxy-cyclohexane with tert.butylamine at 150° C. in an autoclave and then nitrosating the mixture with sodium nitrite/HCl) under a nitrogen atmosphere in the course of 2 days, the mixture being heated at 50° C. The residual lithium alanate is destroyed by cooling the mixture and careful dropwise addition of 50 ml of methanol and then 75 ml of water. The mixture is then filtered and the filtrate is concentrated. The residue is taken up in 100 ml of methylene chloride, the water which separates out is separated off and the organic phase is dried and concentrated again. The oil thus obtainable is dissolved in 20 ml of ethanol and 150 ml of tert.-butyl methyl ether, and the hydrazine hydrochloride is precipitated by addition of ethereal HCl. Yield: 28.5 g melting point: 145° C. (decomp.)

後処理

  1. customobtained
  2. customin the course of 2 days
  3. customThe residual lithium alanate is destroyed
  4. temperatureby cooling
  5. additionthe mixture and careful dropwise addition of 50 ml of methanol
  6. filtrationThe mixture is then filtered
  7. concentrationthe filtrate is concentrated
  8. customthe water which separates out is separated off
  9. customthe organic phase is dried
  10. concentrationconcentrated again
  11. dissolutionThe oil thus obtainable is dissolved in 20 ml of ethanol
  12. custom150 ml of tert.-butyl methyl ether, and the hydrazine hydrochloride is precipitated by addition of ethereal HCl

出典と根拠

ORDレコード
ord-82a32edba3ed413aaf6600e57e63dab3
出典データセット
uspto-grants-1991_04
特許番号
US05006540

関連ノート

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