Sodium Hydroxide → HCID 178478633, 화합물

HRID 1581136노트

반응식

HRID 1581136 반응식
[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]

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 91296N-Methyl-o-phenylenediamine dihydrochlorideHCID 178418324HCID 178418324, 화합물

생성물 1

HCID 178478633HCID 178478633, 화합물수율 42%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-232650ec2c38446eacf20160de375e03
출처 데이터셋
uspto-grants-1976_01
특허 번호
US03935314

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