Sodium Hydroxide → HCID 178478633、化合物

HRID 1581136ノート

反応式

HRID 1581136 の反応式
[ClH:1].Cl.[CH3:3][NH:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1N.[C:12]([NH:14][C:15]([NH2:17])=[NH:16])#[N:13].[OH-].[Na+]>O>[ClH:1].[ClH:1].[NH:14]([C:12]1[N:4]([CH3:3])[C:5]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=2[N:13]=1)[C:15]([NH2:17])=[NH:16]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 91296N-Methyl-o-phenylenediamine dihydrochlorideHCID 178418324HCID 178418324、化合物

生成物 1

HCID 178478633HCID 178478633、化合物収率 42%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of N-methyl-o-phenylenediamine dihydrochloride (10.80g. 0.005 mol) and cyanoguanidine (9.30g, 0.11 mol) was heated under reflux in water (80 ml) for 21/2 hours. The reaction mixture was cooled, basified with excess 40% sodium hydroxide, and the resulting precipitate filtered, washed with water and dried in vacuo. (7.19g; m.p. 142°-146°C). This was dissolved in excess dilute hydrochloric acid and evaporated in vacuo. The crude hydrochloride was recrystallised from ethanol/ether to yield 2-guanidino-1-methylbenzimidazole dihydrochloride (600g; 42%) as off-white micro-crystals m.p. 228°-238°C.

後処理

  1. temperaturewas heated
  2. temperatureThe reaction mixture was cooled
  3. filtrationthe resulting precipitate filtered
  4. washwashed with water
  5. customdried in vacuo
  6. dissolutionThis was dissolved in excess dilute hydrochloric acid
  7. customevaporated in vacuo
  8. customThe crude hydrochloride was recrystallised from ethanol/ether

出典と根拠

ORDレコード
ord-232650ec2c38446eacf20160de375e03
出典データセット
uspto-grants-1976_01
特許番号
US03935314

反応ノート

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