HCID 23002992, 화합물 → HCID 66618157, 화합물

HRID 2093556노트

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HRID 2093556 반응식
[BrH:1].C(O)C.[NH2:5][C:6]1[C:7]2[C:8]3[C:9](=[N:21][N:22]([CH2:24][C:25]4[C:30]([Cl:31])=[C:29]([O:32][CH3:33])[C:28]([CH3:34])=[CH:27][N:26]=4)[N:23]=2)[CH:10]=[C:11]([CH2:16][C:17]([NH:19][CH3:20])=[O:18])[C:12]=3[CH2:13][S:14][N:15]=1>C(#N)C>[BrH:1].[NH2:5][C:6]1[C:7]2[C:8]3[C:9](=[N:21][N:22]([CH2:24][C:25]4[C:30]([Cl:31])=[C:29]([O:32][CH3:33])[C:28]([CH3:34])=[CH:27][N:26]=4)[N:23]=2)[CH:10]=[C:11]([CH2:16][C:17]([NH:19][CH3:20])=[O:18])[C:12]=3[CH2:13][S:14][N:15]=1

참가 물질

4

반응물 2

HCID 23002992HCID 23002992, 화합물HCID 666180742-{4-Amino-2-[(3-chloro-4-methoxy-5-methylpyridin-2-yl)methyl]-2,7-dihydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-8-yl}-N-methylacetamide

생성물 1

HCID 66618157HCID 66618157, 화합물수율 48.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A 20% hydrobromic acid-ethanol solution (204 μl, 0.505 mmol) was added to an acetonitrile solution (350 ml) of 2-{4-amino-2-[(3-chloro-4-methoxy-5-methylpyridin-2-yl)methyl]-2,7-dihydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-8-yl}-N-methylacetamide (250 mg, 0.561 mmol) at room temperature. The resulting mixture was stirred for 3 hours, and the precipitated solid was then collected by filtration. Ethanol (3 ml) was added to the resulting solid, and the resulting mixture was then stirred for 1 day. Thereafter, the solid was collected by filtration. The solid was then dried under reduced pressure at room temperature for 2 days, so as to obtain the title compound (128 mg, 0.243 mmol).

후처리

  1. filtrationthe precipitated solid was then collected by filtration
  2. additionEthanol (3 ml) was added to the resulting solid
  3. stirringthe resulting mixture was then stirred for 1 day
  4. filtrationThereafter, the solid was collected by filtration
  5. customThe solid was then dried under reduced pressure at room temperature for 2 days

출처 및 근거

ORD 기록
ord-de7fd8c92dc3472cb3586667fb2f7e6e
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08445504B2

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