1,2-Dichloroethane → HCID 11649425、化合物

HRID 2244967

反応式

HRID 2244967 の反応式
[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([CH2:11][CH:12]([NH2:16])[C:13]([OH:15])=O)=[CH:3]1.[Cl:17][C:18]1[CH:23]=[CH:22][C:21]([N:24]=[C:25]=[O:26])=[CH:20][CH:19]=1.[CH3:27][N:28]1[CH2:32][CH2:31][N:30]=[C:29]1[C:33]1[CH:38]=[CH:37][C:36]([NH2:39])=[CH:35][CH:34]=1.C(Cl)CCl>CN(C=O)C.O>[CH3:27][N:28]1[CH2:32][CH2:31][N:30]=[C:29]1[C:33]1[CH:38]=[CH:37][C:36]([NH:39][C:13](=[O:15])[CH:12]([CH2:11][C:4]2[C:5]3[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=3)[N:2]([CH3:1])[CH:3]=2)[NH:16][C:25]([NH:24][C:21]2[CH:22]=[CH:23][C:18]([Cl:17])=[CH:19][CH:20]=2)=[O:26])=[CH:35][CH:34]=1

参加物

7

反応物 4

HCID 111,2-DichloroethaneHCID 76934-Chlorophenyl IsocyanateHCID 981121-MethyltryptophanHCID 227288764-(1-Methyl-4,5-dihydro-1H-imidazol-2-yl)-phenylamine

生成物 1

HCID 11649425HCID 11649425、化合物収率 61.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution of DL-1-methyl-tryptophan (71 mg, 0.33 mmol) in DMF (4 mL), 4-chlorophenyl isocyanate (50 mg, 0.33 mmol) was added. The mixture was then stirred at room temperature overnight. It was filtered. To the filtrate, 4-(1-Methyl-4,5-dihydro-1H-imidazol-2-yl)-phenylamine (150 mg, 0.86 mmol) and H2O (0.5 mL, to solubilize the amine) were added. To the solution, EDC (127 mg, 0.66 mmol) was added. After being stirred at room temperature overnight, the solution was concentrated in vacuo. The residue was purified by HPLC to give the titled compound as a powder (108 mg). MS 529.2 and 531.2 (M+H, Cl pattern).

後処理

  1. filtrationIt was filtered
  2. additionwere added
  3. stirringAfter being stirred at room temperature overnight
  4. concentrationthe solution was concentrated in vacuo
  5. customThe residue was purified by HPLC

出典と根拠

ORDレコード
ord-aaf74f853ba04c9a9f7b0d724e2dd667
出典データセット
uspto-grants-2010_03
特許番号
US07678913B2

関連ノート

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