Hydrochloric Acid → HCID 178419031、化合物

HRID 6853

反応式

HRID 6853 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([NH2:15])[CH:12]=[CH:13][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N:16]#[C:17][NH2:18].Cl.[OH-].[Na+]>O1CCOCC1>[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([NH:15][C:17]([NH2:18])=[NH:16])[CH:12]=[CH:13][CH:14]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 9864CyanamideHCID 14798Sodium HydroxideHCID 928923-Benzyloxyaniline

生成物 1

HCID 178419031HCID 178419031、化合物収率 98.4%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

反応条件

温度
80 °C

実験手順

To a suspension of 3-benzyloxyphenylamine (20.0 g, 100.35 mmol) in 1,4-dioxane (150 mL) was added cyanamide (7.39 g, 175.95 mmol followed by 4M HCl in 1,4-dioxane (44 ml, 176.00 mmol). The resulting suspension was heated at 80° C. overnight then cooled to ambient temperature and 6N NaOH (35 ml, 210.00 mmol) was added. The volume of solution was reduced to 50 ml in vacuo and the resulting precipitate was collected by filtration. The solid product was dried under vacuum overnight to afford 23.8 g in 98.4% yield. 1H NMR (MeOH-d4) δ 6.4–7.5 (m, 9H), 5.1 (s, 2H).

後処理

  1. temperaturethen cooled to ambient temperature
  2. filtrationthe resulting precipitate was collected by filtration
  3. customThe solid product was dried under vacuum overnight
  4. customto afford 23.8 g in 98.4% yield

出典と根拠

ORDレコード
ord-e6b1f13036c244b682cb1d3247b19d66
出典データセット
uspto-grants-2006_08
特許番号
US07084159B2

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