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

HRID 1697288

반응식

HRID 1697288 반응식
[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

참가 물질

4

반응물 3

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

생성물 1

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

반응 조건

온도
100 °C

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-960619c4624647feb22b610c1cf95e28
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08163905B2

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