Tert-Butylamine → HCID 14795576, 화합물

HRID 1084784

반응식

HRID 1084784 반응식
[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]

참가 물질

6

반응물 5

HCID 6385Tert-ButylamineHCID 9246Cyclohexene oxideHCID 3028194LithiumHCID 21652828HCID 21652828, 화합물HCID 86602196Hydrochloride sodium nitrite

생성물 1

HCID 14795576HCID 14795576, 화합물

반응 조건

온도
50 °C

실험 절차

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.)

후처리

  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

출처 및 근거

ORD 기록
ord-82a32edba3ed413aaf6600e57e63dab3
출처 데이터셋
uspto-grants-1991_04
특허 번호
US05006540

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