Diisopropylethylamine → HCID 86634073, 화합물

HRID 1041723노트

반응식

HRID 1041723 반응식
[NH2:1][C:2]1[C:10]([CH3:11])=[CH:9][C:8]([CH3:12])=[CH:7][C:3]=1[C:4]([NH2:6])=[O:5].[CH3:13]CN(C(C)C)C(C)C.[Cl:22][C:23]1[N:28]=[C:27](Cl)[C:26]([Cl:30])=[CH:25][N:24]=1>CS(C)=O.C(Cl)Cl>[Cl:22][C:23]1[N:28]=[C:27]([NH:1][C:2]2[C:10]([CH3:11])=[CH:9][C:8]([CH3:12])=[CH:7][C:3]=2[C:4]([NH:6][CH3:13])=[O:5])[C:26]([Cl:30])=[CH:25][N:24]=1

참가 물질

6

반응물 3

HCID 81531DiisopropylethylamineHCID 2372592,4,5-TrichloropyrimidineHCID 122648222-Amino-3,5-dimethylbenzamide

생성물 1

HCID 86634073HCID 86634073, 화합물

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 6344Dichloromethane용매

실험 절차

A solution of 2-amino-3,5-dimethyl-benzamide (573 mg), DIEA (580 mL), and 2,4,5-trichloropyrimidine (660 mg) in DMSO was heated at 65° C. for 4.5 h, then diluted with DCM, washed with brine twice, dried over sodium sulfate, and concentrated in vacuo. The residue was purified by silica gel chromatography to provide 460 mg of 2-(2,5-dichloropyrimidin-4-ylamino)-3,5,N-trimethyl-benzamide: 1H NMR (300 MHz, CDCl3) δ 9.3 (bs, 1H), 8.2 (s, 1H), 7.3 (s, 1H), 7.2 (s, 1H), 6.2 (bs, 1H), 3.0 (d, 3H), 2.4 (s, 3H), 2.3 (s, 3H).

후처리

  1. washwashed with brine twice
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-f1799136b0b143188195167651e089ce
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08552186B2

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