Acetonitrile → HCID 136388339, 화합물

HRID 1861943노트

반응식

HRID 1861943 반응식
[C:1]([O:5][C:6](=[O:18])[NH:7][CH2:8][C:9]1[CH:14]=[C:13]([NH2:15])[CH:12]=[CH:11][C:10]=1[O:16][CH3:17])([CH3:4])([CH3:3])[CH3:2].C(N(CC)CC)C.CS[C:28](=[NH:33])[NH:29][N+:30]([O-:32])=[O:31].C(#N)C>CO>[C:1]([O:5][C:6](=[O:18])[NH:7][CH2:8][C:9]1[CH:14]=[C:13]([NH:15][C:28]([NH2:33])=[N:29][N+:30]([O-:32])=[O:31])[CH:12]=[CH:11][C:10]=1[O:16][CH3:17])([CH3:4])([CH3:3])[CH3:2]

참가 물질

6

반응물 4

HCID 6342AcetonitrileHCID 8471TriethylamineHCID 22981333Tert-butyl 5-amino-2-methoxybenzylcarbamateHCID 135927615N-Nitro-S-methylisothiourea

생성물 1

HCID 136388339HCID 136388339, 화합물수율 33%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of the compound (130 mg) obtained in Example 119, triethylamine (0.09 ml), S-methyl-N-nitroisothiourea (84 mg), acetonitrile (3 ml) and methanol (1 ml) was heated under reflux for 20 h. The reaction mixture was distilled under reduced pressure and the residue was purified by silica gel column chromatography (eluent, chloroform:ethyl acetate=1:1) to give 57.2 mg of the titled compound (yield, 33%).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 20 h
  3. distillationThe reaction mixture was distilled under reduced pressure
  4. customthe residue was purified by silica gel column chromatography (eluent, chloroform:ethyl acetate=1:1)

출처 및 근거

ORD 기록
ord-328f610d947645a4a0b69322f0c8c1e6
출처 데이터셋
uspto-grants-2003_03
특허 번호
US06534546B1

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