Hydrochloric Acid → HCID 12508676, 화합물

HRID 1633331노트

반응식

HRID 1633331 반응식
[CH2:1]([C:6]1([CH3:18])[CH:11]([CH2:12][CH3:13])[NH:10]C(CC)[NH:8][CH:7]1[CH2:16][CH3:17])[NH:2][CH2:3][CH2:4][CH3:5].Cl>O>[NH2:8][CH:7]([CH2:16][CH3:17])[C:6]([CH:11]([NH2:10])[CH2:12][CH3:13])([CH3:18])[CH2:1][NH:2][CH2:3][CH2:4][CH3:5]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 12508669HCID 12508669, 화합물

생성물 1

HCID 12508676HCID 12508676, 화합물수율 84.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 21.1 grams of 5-(2-azapentyl)-5-methyl-2,4,6-triethylhexahydropyrimidine, prepared as described in example 1, 25 grams of conc. HCl and 25 grams of water was refluxed for 2 hours. The organic layer which separated was removed and discarded and the aqueous solution after extraction with ether was basified with a sodium hydroxide solution. The organic layer which separated was removed and the aqueous phase extracted with ether. The ethereal solution was combined with the organic layer and after drying evaporated under diminished pressure to yield 15.0 grams of 7-amino-6-(1-aminopropyl)-6-methyl-4-azanonane; b.p. 72°-76° C./0.05 torr; Infrared spectrum, 2.97 and 3.05μ (N-H) and 6.15μ (NH2); 'H nuclear magnetic resonance spectrum, solvent CDCl3, internal reference tetramethylsilane, δ in ppm: 3.07-2.30, 6H; 2.00-1.14, 6H; 1.14-0.67, 12H. 13C nuclear magnetic resonance spectrum, solvent CDCl3, internal reference tetramethylsilane, δ in ppm: ##STR7## 11.9(1); 23.2(2); 52.9 and 52.8(3); 54.7 and 54.3(5); 42.9 and 43.1(6); 58.8, 56.7 and 57.5(7,11); 24.9, 24.7 and 25.7(8,12); 12.2(9,13); 19.2 and 17.0(10).

후처리

  1. customprepared
  2. temperaturewas refluxed for 2 hours
  3. customThe organic layer which separated
  4. customwas removed
  5. extractionthe aqueous solution after extraction with ether
  6. customThe organic layer which separated
  7. customwas removed
  8. extractionthe aqueous phase extracted with ether
  9. customafter drying
  10. customevaporated under diminished pressure

출처 및 근거

ORD 기록
ord-ac4d271be91246adbf866109c4661d80
출처 데이터셋
uspto-grants-1984_10
특허 번호
US04480095

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