Triethylamine → HCID 25169485, 화합물

HRID 1514346노트

반응식

HRID 1514346 반응식
[CH3:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][CH:7]=[N:8]2)=[C:4](Cl)[N:3]=1.[CH3:12][O:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([NH2:20])[CH:15]=1.C(N(CC)CC)C>C(O)CCC>[CH3:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][CH:7]=[N:8]2)=[C:4]([NH:20][C:16]2[CH:17]=[CH:18][CH:19]=[C:14]([O:13][CH3:12])[CH:15]=2)[N:3]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 108243-MethoxyanilineHCID 54089976-chloro-2-methyl-7H-purine

생성물 1

HCID 25169485HCID 25169485, 화합물

시약·촉매·용매 1

HCID 2631-Butanol용매

반응 조건

온도
110 °C

실험 절차

To a suspension of 2-methyl-6-chloropurine (1.69 g; 0.01 mol) and m-anisidine (1.23 g; 0.01 mol) in n-butanol (20 ml), triethylamine (3.5 ml; 0.025 mol) was added. The resulting thick suspension was stirred at 110° C. for 3 hours, when TLC showed the absence of starting material and the presence of desired product. The reaction mixture was then cooled to room temperature. The white precipitate was filtered off, rinsed with n-butanol (2×10 ml) and water (3×10 ml) and dried into constant weight. Yield: 1.92 g (75%). The crude product was purified as hydrochloride salt by the crystallization from 2.5 M methanolic hydrochloric acid. TLC (chloroform-methanol-NH4OH; 4:1:0.05): one single spot, free of starting material. HPLC purity: 99+%.

후처리

  1. additionwas added

출처 및 근거

ORD 기록
ord-1c09d6a7f4584c518bed9aaf5fdea036
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08222260B2

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