Hydrochloric Acid → HCID 178493227、化合物

HRID 1930597

反応式

HRID 1930597 の反応式
Cl.[CH3:2][O:3][C:4]1[CH:5]=[C:6]([CH:8]=[CH:9][C:10]=1[N:11]1[CH:15]=[C:14]([CH3:16])[N:13]=[CH:12]1)[NH2:7].[N:17]#[C:18][NH2:19].Cl>C(O)C.O>[CH3:2][O:3][C:4]1[CH:5]=[C:6]([NH:7][C:18]([NH2:19])=[NH:17])[CH:8]=[CH:9][C:10]=1[N:11]1[CH:15]=[C:14]([CH3:16])[N:13]=[CH:12]1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 9864CyanamideHCID 674242353-Methoxy-4-(4-methyl-1H-imidazol-1-yl)aniline hydrochloride

生成物 1

HCID 178493227HCID 178493227、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

3-Methoxy-4-(4-methyl-1H-imidazol-1-yl)aniline hydrochloride (3 g, 12.52 mmol), cyanamide (0.684 g, 16.27 mmol) and hydrochloric acid (1.564 mL, 18.77 mmol) in ethanol (20 mL) were heated to reflux o.n. The reaction mixture was concentrated under reduced pressure before the residue was poured on potassium carbonate (1.730 g, 12.52 mmol) in water (60 mL) and then put in refrigerator o.n. The formed carbonate-salt was filtered off, and dried in vacuum oven o.n. The solid was washed with several portions of DCM, dried and used as such in next step (52.3%). MS (ES+) m/z 246.2 (M+H)+

後処理

  1. temperatureto reflux o.n
  2. concentrationThe reaction mixture was concentrated under reduced pressure before the residue
  3. filtrationThe formed carbonate-salt was filtered off
  4. customdried in vacuum oven o.n
  5. washThe solid was washed with several portions of DCM
  6. customdried

出典と根拠

ORDレコード
ord-747b10de2d1d40299d4b993bc021f52f
出典データセット
uspto-grants-2012_05
特許番号
US08188101B2

関連ノート

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