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N-methyl-2-pyrrolidone → HCID 67212942, 화합물

HRID 2223826
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HRID 2223826 반응식
[F:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6][NH2:7])=[CH:4][CH:3]=1.C(N(C(C)C)CC)(C)C.CN1CCCC1=O.Cl[C:27]1[N:32]=[C:31]([NH:33][C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[N:30]=[C:29]([NH:40][C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)[N:28]=1>C(#N)C>[C:41]1([NH:40][C:29]2[N:30]=[C:31]([NH:33][C:34]3[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=3)[N:32]=[C:27]([NH:7][CH2:6][C:5]3[CH:8]=[CH:9][C:2]([F:1])=[CH:3][CH:4]=3)[N:28]=2)[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 13387N-methyl-2-pyrrolidoneHCID 160881,3,5-Triazine-2,4-diamine, 6-chloro-N2,N4-diphenyl-HCID 673264-FluorobenzylamineHCID 81531Diisopropylethylamine

생성물 1

HCID 67212942HCID 67212942, 화합물수율 45%

시약·촉매·용매 1

HCID 6342Acetonitrile
용매

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온도
80 °C

실험 절차

A 7.5 mg (60 μmol) portion of p-fluorobenzylamine and 52 μl of diisopropylethylamine were added to a mixed solution of 400 μl of acetonitrile and 120 μl of N-methylpyrrolidone containing 8.9 mg (30 μmol) of 6-chloro-N,N′-diphenyl-1,3,5-triazine-2,4-diamine and stirred at 80° C. for 3 hours. The reaction solution was filtered and then injected into a fractional LC-MS apparatus to collect a fraction containing the desired molecular weight. By evaporating the solvent, 6.1 mg (yield 45%) of N,N′-diphenyl-N″-(4-fluorobenzyl)-1,3,5-triazine-2,4,6-triamine was obtained. A retention time of 2.77 minutes and a purity of 93% were determined by an analytical LC-MS.

후처리

  1. filtrationThe reaction solution was filtered
  2. customto collect a fraction
  3. additioncontaining the desired molecular weight
  4. customBy evaporating the solvent

출처 및 근거

ORD 기록
ord-dd3c4e2ce9c745afb0130eac81ff7091
출처 데이터셋
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07375222B2

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