Ethylamine → 4-Amino-N-(2-amino-6-ethylamino-pyrimidin-4-yl)-benzenesufonamide

HRID 1584172노트

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HRID 1584172 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12]2[CH:17]=[C:16](Cl)[N:15]=[C:14]([NH2:19])[N:13]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.[CH2:20]([NH2:22])[CH3:21]>C(O)C>[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12]2[CH:17]=[C:16]([NH:22][CH2:20][CH3:21])[N:15]=[C:14]([NH2:19])[N:13]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 6341EthylamineHCID 107329394-amino-N-(2-amino-6-chloro-pyrimidin-4-yl)-benzenesulfonamide

생성물 1

HCID 107335984-Amino-N-(2-amino-6-ethylamino-pyrimidin-4-yl)-benzenesufonamide수율 53%

시약·촉매·용매 1

HCID 702Ethanol용매2회

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온도
130 °C

실험 절차

0.50 g (0.00167 mol) of 4-amino-N-(2-amino-6-chloro-pyrimidin-4-yl)-benzenesufonamide and 11 ml (0.167 mol) of ethylamine were dissolved in 20 ml of ethanol and stirred in an autoclave at 130° C. for 4 hours. The reaction mixture was freed from solvent, the residue was suspended in 5 ml of ethanol and treated in an ultrasound bath for 15 minutes. The precipitate was filtered off, dissolved 10 ml of 0.1N NaOH and filtered. The filtrate was adjusted to pH 6 with 0.1N HCl. The precipitate was filtered off under suction, washed with water and dried. There was obtained 0.271 g (53%) of 4-amino-N-(2-amino-6-ethylamino-pyrimidin-4-yl)-benzenesulfonamide as beige crystals; m.p. 272-274° C.

후처리

  1. additiontreated in an ultrasound bath for 15 minutes
  2. filtrationThe precipitate was filtered off
  3. dissolutiondissolved 10 ml of 0.1N NaOH
  4. filtrationfiltered
  5. filtrationThe precipitate was filtered off under suction
  6. washwashed with water
  7. customdried

출처 및 근거

ORD 기록
ord-7e864cc3a0354b42a2605b5468a37021
출처 데이터셋
uspto-grants-1999_08
특허 번호
US05932599

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