Methyl iodide → HCID 23287658, 화합물

HRID 367120노트

반응식

HRID 367120 반응식
[Br:1][C:2]1[CH:19]=[CH:18][C:5]([NH:6][C:7]2[S:8][C:9]3[N:17]=[CH:16][CH:15]=[CH:14][C:10]=3[C:11](=[O:13])[N:12]=2)=[CH:4][CH:3]=1.[H-].[Li+].[CH3:22]I>>[Br:1][C:2]1[CH:19]=[CH:18][C:5]([N:6]=[C:7]2[N:12]([CH3:22])[C:11](=[O:13])[C:10]3[CH:14]=[CH:15][CH:16]=[N:17][C:9]=3[S:8]2)=[CH:4][CH:3]=1

참가 물질

4

반응물 3

HCID 6328Methyl iodideHCID 62714Lithium hydrideHCID 52306034H-Pyrido[3,2-e]-1,3-thiazin-4-one, 2-[(4-bromophenyl)amino]-

생성물 1

HCID 23287658HCID 23287658, 화합물수율 85.7%

실험 절차

The reaction procedure of Example 11 was followed except that 900 mg (2.69 mmol) of 2-(4-bromoanilino)-4H-pyrido[3,2-e]-1,3-thiazin-4-one, 24 mg of lithium hydride and =420 mg of methyl iodide were used. The resulting residue was then purified through silica gel column chromatography (eluant: chloroform) to obtain 803 mg of 2-[(4-bromophenyl)imino]-2,3-dihydro-3-methyl-4H-pyrido[3,2-e]-1,3-thiazin-4-one (86%, recrystallized from a mixture of ether and hexane) as a low polarity substance and 107 mg of 2-[N-(4-bromophenyl)-N-methylamino]-4H-pyrido[3,2-e]-1,3-thiazin-4-one (recrystallized from ether) as a high polarity substance.

후처리

  1. customThe reaction procedure of Example 11
  2. customThe resulting residue was then purified through silica gel column chromatography (eluant: chloroform)

출처 및 근거

ORD 기록
ord-b063e2490dc44394b7790180245ce0f7
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06133258

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