1,2-Dichlorobenzene → 3-(3,5-Dichloro-2-oxo-1(2H)-pyrazinyl)-4-methyl-benzoic acid, methyl ester

HRID 337028ノート

反応式

HRID 337028 の反応式
[C:1]([CH2:3][NH:4][C:5]1[CH:6]=[C:7]([CH:12]=[CH:13][C:14]=1[CH3:15])[C:8]([O:10][CH3:11])=[O:9])#[N:2].[C:16]([Cl:21])(=O)[C:17](Cl)=[O:18].[Cl:22]C1C=CC=CC=1Cl>>[Cl:21][C:16]1[C:17](=[O:18])[N:4]([C:5]2[CH:6]=[C:7]([CH:12]=[CH:13][C:14]=2[CH3:15])[C:8]([O:10][CH3:11])=[O:9])[CH:3]=[C:1]([Cl:22])[N:2]=1

参加物

4

反応物 3

HCID 72391,2-DichlorobenzeneHCID 65578Oxalyl chlorideHCID 86663236Methyl 3-[(cyanomethyl)amino]-4-methylbenzoate

生成物 1

HCID 866632353-(3,5-Dichloro-2-oxo-1(2H)-pyrazinyl)-4-methyl-benzoic acid, methyl ester

反応条件

温度
100 °C

実験手順

To 3-[(cyanomethyl)amino]-4-methyl-benzoic acid, methyl ester (Example 1a, 1.2 g) was added 1,2-dichlorobenzene (20 mL) and oxalyl chloride (3 mL). The reaction was heated at 100° C. for four h before the volatiles were removed under reduced pressure. The residue was purified (SiO2 chromatography eluting with dichloromethane) to afford the subtitle compound (800 mg).

後処理

  1. customwere removed under reduced pressure
  2. customThe residue was purified
  3. wash(SiO2 chromatography eluting with dichloromethane)

出典と根拠

ORDレコード
ord-c4787786d5a94a10adaa88c2df464856
出典データセット
uspto-grants-2014_11
特許番号
US08889692B2

反応ノート

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