Toluene → HCID 135984689、化合物

HRID 249778ノート

反応式

HRID 249778 の反応式
[CH3:1][C:2]1[N:6]=[C:5]([C:7]2[NH:11][CH:10]=[N:9][C:8]=2[NH:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[NH:4][N:3]=1.[C:18](Cl)(Cl)=[O:19].C1(C)C=CC=CC=1>C1COCC1>[CH3:1][C:2]1[N:6]=[C:5]2[N:4]([C:18](=[O:19])[N:12]([CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[C:8]3[N:9]=[CH:10][NH:11][C:7]=32)[N:3]=1

参加物

5

反応物 3

HCID 1140TolueneHCID 6371PhosgeneHCID 178446281HCID 178446281、化合物

生成物 1

HCID 135984689HCID 135984689、化合物収率 50%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 5-(3-methyl-1H-1,2,4-triazol-5-yl)-N-pentyl-1H-imidazol-4-amine (45 mg, 0.19 mmol) in THF (10 mL) at 0° C. was added phosgene in toluene (0.3 mL, 1.0 mmol). The reaction mixture was slowly warmed to room temperature while stirring. The reaction mixture was concentrated under reduced pressure, and the residue was purified by preparative LCMS (method A) to provide the desired product (25 mg, 50% yield) as a white powder. LCMS calculated for C12H17N6O (M+H): 261.1. found: 261.1.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe residue was purified by preparative LCMS (method A)

出典と根拠

ORDレコード
ord-391e741a0cfa42b690a3931b4e111156
出典データセット
uspto-grants-2011_01
特許番号
US07863285B2

反応ノート

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