Triethylamine → 2-Chloro-4-[3-(3-nitro-benzenesulfonylamino)-propylamino]-pyrimidine-5-carboxylic acid-tert-butylamide

HRID 970425

반응식

HRID 970425 반응식
[C:1]([NH:5][C:6]([C:8]1[C:9](Cl)=[N:10][C:11]([Cl:14])=[N:12][CH:13]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[NH2:16][CH2:17][CH2:18][CH2:19][NH:20][S:21]([C:24]1[CH:29]=[CH:28][CH:27]=[C:26]([N+:30]([O-:32])=[O:31])[CH:25]=1)(=[O:23])=[O:22].C(N(CC)CC)C>C1COCC1>[C:1]([NH:5][C:6]([C:8]1[C:9]([NH:16][CH2:17][CH2:18][CH2:19][NH:20][S:21]([C:24]2[CH:29]=[CH:28][CH:27]=[C:26]([N+:30]([O-:32])=[O:31])[CH:25]=2)(=[O:22])=[O:23])=[N:10][C:11]([Cl:14])=[N:12][CH:13]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 223267522,4-Dichloro-pyrimidine-5-carboxylic acid-tert-butylamideHCID 24711458N-(3-amino-propyl)-3-nitro-benzenesulfonamide

생성물 1

HCID 590203532-Chloro-4-[3-(3-nitro-benzenesulfonylamino)-propylamino]-pyrimidine-5-carboxylic acid-tert-butylamide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 0.95 g (3.83 mmol) of 2,4-dichloro-pyrimidine-5-carboxylic acid-tert-butylamide in 6 ml of THF is mixed at room temperature while being stirred with a suspension that consists of 1.00 g (3.86 mmol) of N-(3-amino-propyl)-3-nitro-benzenesulfonamide in 9 ml of THF/0.55 ml of triethylamine. After 19 hours, the precipitate that is formed is suctioned off and washed with ethyl acetate. The filtrate is spun in, and the residue that is formed is purified by chromatography (hexane/ethyl acetate 2:1, Flashmaster II). 0.79 g (1.67 mmol, corresponding to 44% of theory) of the product is obtained.

후처리

  1. customthe precipitate that is formed
  2. washwashed with ethyl acetate
  3. customis formed
  4. customis purified by chromatography (hexane/ethyl acetate 2:1, Flashmaster II)
  5. custom0.79 g (1.67 mmol, corresponding to 44% of theory) of the product is obtained

출처 및 근거

ORD 기록
ord-0db5b4a523594f119ebe43eb544973a3
출처 데이터셋
uspto-grants-2007_12
특허 번호
US07312225B2

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