Diethyl Ether → HCID 86652177、化合物

HRID 2093558ノート

反応式

HRID 2093558 の反応式
C(OCC)C.[CH3:6][S:7]([OH:10])(=[O:9])=[O:8].[NH2:11][C:12]1[C:13]2[C:14]3[C:15](=[N:27][N:28]([CH2:30][C:31]4[C:36]([Cl:37])=[C:35]([O:38][CH3:39])[C:34]([CH3:40])=[CH:33][N:32]=4)[N:29]=2)[CH:16]=[C:17]([CH2:22][C:23]([NH:25][CH3:26])=[O:24])[C:18]=3[CH2:19][S:20][N:21]=1>C(#N)C>[CH3:6][S:7]([OH:10])(=[O:9])=[O:8].[NH2:11][C:12]1[C:13]2[C:14]3[C:15](=[N:27][N:28]([CH2:30][C:31]4[C:36]([Cl:37])=[C:35]([O:38][CH3:39])[C:34]([CH3:40])=[CH:33][N:32]=4)[N:29]=2)[CH:16]=[C:17]([CH2:22][C:23]([NH:25][CH3:26])=[O:24])[C:18]=3[CH2:19][S:20][N:21]=1

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 6395Methanesulfonic AcidHCID 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

生成物 1

HCID 86652177HCID 86652177、化合物収率 88.7%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
5 °C

実験手順

A diethyl ether solution (50 ml) of methanesulfonic acid (32 mg, 0.302 mmol) was added at 5° C. to an acetonitrile solution (150 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 (151 mg, 0.339 mmol). The resulting mixture was stirred at 5° C. for 25 minutes. Thereafter, the solvent was distilled away under reduced pressure, an appropriate amount of diethyl ether was then added to the residue, and a solid was then collected by filtration. Thereafter, ethanol (1 ml) was added to the resulting solid, and the resulting mixture was then stirred at room temperature for approximately 1 day. Thereafter, a solid was collected by filtration, and it was then dried under reduced pressure at room temperature for 1 day, so as to obtain the title compound (145 mg, 0.268 mmol).

後処理

  1. distillationThereafter, the solvent was distilled away under reduced pressure
  2. additionan appropriate amount of diethyl ether was then added to the residue
  3. filtrationa solid was then collected by filtration
  4. additionThereafter, ethanol (1 ml) was added to the resulting solid
  5. stirringthe resulting mixture was then stirred at room temperature for approximately 1 day
  6. filtrationThereafter, a solid was collected by filtration, and it
  7. customwas then dried under reduced pressure at room temperature for 1 day

出典と根拠

ORDレコード
ord-78ceabf0b5684ae6889c2be4d9218c89
出典データセット
uspto-grants-2013_05
特許番号
US08445504B2

反応ノート

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