Acetonitrile → HCID 136388339、化合物

HRID 1861943ノート

反応式

HRID 1861943 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 136388339HCID 136388339、化合物収率 33%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-328f610d947645a4a0b69322f0c8c1e6
出典データセット
uspto-grants-2003_03
特許番号
US06534546B1

反応ノート

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