Triethylamine → {5-[4-Amino-6-(2-methoxy-phenylsulfanyl)-[1,3,5]triazin-2-yl]-2,4-dichlorophenoxy}-acetonitrile

HRID 217282

反応式

C(N(CC)CC)C.[CH3:8][O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[SH:16].[NH2:17][C:18]1[N:23]=[C:22](S(CC2C=CC=CC=2)=O)[N:21]=[C:20]([C:33]2[C:34]([Cl:44])=[CH:35][C:36]([Cl:43])=[C:37]([CH:42]=2)[O:38][CH2:39][C:40]#[N:41])[N:19]=1>CN(C)C=O>[NH2:17][C:18]1[N:23]=[C:22]([S:16][C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[O:9][CH3:8])[N:21]=[C:20]([C:33]2[C:34]([Cl:44])=[CH:35][C:36]([Cl:43])=[C:37]([CH:42]=2)[O:38][CH2:39][C:40]#[N:41])[N:19]=1

参加物

実験手順

Triethylamine (12 μL) and 2-methoxybenzenethiol (12 mg) were added in succession to a solution of the above-described [5-(4-amino-6-phenylmethanesulfinyl-[1,3,5]triazin-2-yl)-2,4-dichlorophenoxy]-acetonitrile (12 mg) in dimethylformamide (0.5 mL). The mixture was stirred at room temperature for 8 hours. After dilution with ethyl acetate (7 mL), the mixture was washed twice with water and once with brine. The mixture was pre-dried over anhydrous sodium sulfate, and filtered. The solvent was distilled off. The resulting residue was purified by silica gel column chromatography (developing solvent: hexane:ethyl acetate=7:3) to give {5-[4-amino-6-(2-methoxy-phenylsulfanyl)-[1,3,5]triazin-2-yl]-2,4-dichlorophenoxy}-acetonitrile as white solid (10 mg).

後処理

washAfter dilution with ethyl acetate (7 mL), the mixture was washed twice with water and once with brine
dry with materialThe mixture was pre-dried over anhydrous sodium sulfate
filtrationfiltered
distillationThe solvent was distilled off
customThe resulting residue was purified by silica gel column chromatography (developing solvent: hexane:ethyl acetate=7:3)

出典と根拠

ORDレコード: ord-ef965fb2a051411791d949e5a75fcaf6
出典データセット: uspto-grants-2012_06
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08193351B2

反応式

参加物

反応物 3

生成物 1

試薬・触媒・溶媒 1

実験手順

後処理

出典と根拠

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