Sodium Hydroxide → HCID 13251820, 화합물

HRID 745484

반응식

HRID 745484 반응식
[NH2:1][C@@H:2]1[CH2:7][CH2:6][CH2:5][CH2:4][C@H:3]1[NH2:8].[C:9]([C:13]1[CH:18]=[CH:17][C:16]([CH2:19][CH:20]([CH3:23])[CH2:21]Cl)=[CH:15][CH:14]=1)([CH3:12])([CH3:11])[CH3:10].[OH-].[Na+]>CCOCC>[C:9]([C:13]1[CH:14]=[CH:15][C:16]([CH2:19][CH:20]([CH3:23])[CH2:21][NH:1][C@@H:2]2[CH2:7][CH2:6][CH2:5][CH2:4][C@H:3]2[NH2:8])=[CH:17][CH:18]=1)([CH3:12])([CH3:11])[CH3:10]

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 438061,2-Diaminocyclohexane, trans-HCID 132518171-tert-Butyl-4-(3-chloro-2-methylpropyl)benzene

생성물 1

HCID 13251820HCID 13251820, 화합물수율 83.5%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
140 °C

실험 절차

274 g of trans-1,2-diaminocyclohexane and 134.4 g of 3-(4-tert.-butylphenyl)-2-methylpropyl chloride (German Laid-Open Application DOS No. 2,752,096) were stirred for 10 hours at 140° C. and then cooled to +10° C. in an ice bath, and 200 ml of a 50% strength by weight sodium hydroxide solution were added slowly, followed by the addition of 200 ml of ether. The organic phase was separated off, dried over potassium hydroxide and distilled to give 151 g of N-(3-(4-tert.-butylphenyl)-2-methylpropyl)-trans-1,2-diaminocyclohexane of boiling point 175°-180° C./0.3 mbar. Yield: 83.3% of theory.

후처리

  1. temperaturecooled to +10° C. in an ice bath
  2. customThe organic phase was separated off
  3. dry with materialdried over potassium hydroxide
  4. distillationdistilled

출처 및 근거

ORD 기록
ord-9d6febe3472e4acb8c5384b0ade92637
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04599335

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