Methyl Isocyanate → HCID 10390966、化合物

HRID 374057

反応式

HRID 374057 の反応式
[C:1]1([C:7]2[N:8]=[C:9]([S:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][NH:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])[NH:10][C:11]=2[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:32][N:33]=[C:34]=[O:35]>CCCCCC>[C:1]1([C:7]2[N:8]=[C:9]([S:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][N:24]([CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])[C:34]([NH:33][CH3:32])=[O:35])[NH:10][C:11]=2[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 12228Methyl IsocyanateHCID 10048624N-[5-(4,5-diphenyl-1H-imidazol-2-ylthio)pentyl]-heptanamine

生成物 1

HCID 10390966HCID 10390966、化合物収率 67.1%

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

To a solution of N-[5-(4,5-diphenyl-1H-imidazol-2-ylthio)pentyl]-1-heptanamine (0.30 g, 0.0007 mol) in hexane (15 mL) was added methylisocyanate (0.06 mL, 0.057 g, 0.001 mol) and the reaction mixture was stirred at ambient temperature for 18 hours. The reaction mixture was concentrated under vacuum and the residue was chromatographed with 1:1 hexane-ethyl acetate. The resulting oil was triturated with hexane to give the title compound (0.23 g, 0.00047 mol) as a white solid, mp 93°-96°. 1H NMR (CDCl3) δ7.6-7.2(m,11H), 4.35-2.7(m,9H), 1.9-1.2(m,16H), 0.9(t,3H,J=8Hz).

後処理

  1. concentrationThe reaction mixture was concentrated under vacuum
  2. customthe residue was chromatographed with 1:1 hexane-ethyl acetate
  3. customThe resulting oil was triturated with hexane

出典と根拠

ORDレコード
ord-7fbf014c12194398ab3d5a592a2a4fd4
出典データセット
uspto-grants-1992_11
特許番号
US05166214

関連ノート

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