Hydrochloric Acid → HCID 67768990, 화합물

HRID 1898913노트

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HRID 1898913 반응식
[ClH:1].[CH2:2]([N:4]([C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([C:28]([F:31])([F:30])[F:29])[CH:23]=1)[C:5]([C:7]1[C:8]([NH2:21])=[N:9][C:10]([N:13]2[CH2:17][C:16]([CH3:19])([CH3:18])[NH:15][C:14]2=[O:20])=[N:11][CH:12]=1)=[O:6])[CH3:3]>CCOCC.CC(C)=O>[ClH:1].[CH2:2]([N:4]([C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([C:28]([F:31])([F:29])[F:30])[CH:23]=1)[C:5]([C:7]1[C:8]([NH2:21])=[N:9][C:10]([N:13]2[CH2:17][C:16]([CH3:19])([CH3:18])[NH:15][C:14]2=[O:20])=[N:11][CH:12]=1)=[O:6])[CH3:3]

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 3086669Opanixil

생성물 1

HCID 67768990HCID 67768990, 화합물수율 92.7%

시약·촉매·용매 2

HCID 180Acetone용매HCID 3283Diethyl Ether용매

실험 절차

1.52 ml of a 6.6 molar solution of HCl in ether were added dropwise to a solution of 3.80 g (9 mmol) of 4-amino-2-(4,4-dimethyl-2-oxo-1-imidazolidinyl)-pyrimidine-5-carboxylic acid N-ethyl-N-(3-trifluoromethylphenyl)amide prepared as in Example 1 in 20 ml of acetone at room temperature, and the resulting suspension was stirred while cooling in ice for 20 minutes. The crystals were then filtered off with suction, washed with acetone and ether and dried in vacuo (6-7 mbar) at 100° for 10 hours. 3.83 g (=92.7% yield) of 4-amino-2-(4,4-dimethyl-2-oxo-1-imidazolidinyl)pyrimidine-5-carboxylic acid N-ethyl-N-(3-trifluoromethylphenyl)amide hydrochloride were obtained, melting point 264°-265° (decomposition).

후처리

  1. temperaturewhile cooling in ice for 20 minutes
  2. filtrationThe crystals were then filtered off with suction
  3. washwashed with acetone and ether
  4. customdried in vacuo (6-7 mbar) at 100° for 10 hours

출처 및 근거

ORD 기록
ord-2fbe8d7b3297448b9d2576725e81a436
출처 데이터셋
uspto-grants-1996_11
특허 번호
US05571816

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