1-Naphthalenamine, hydrochloride (1:1) → HCID 178436383、化合物

HRID 257664

反応式

HRID 257664 の反応式
[CH2:1]([C:3]1[CH:4]=[C:5]([N:9]([CH3:12])[C:10]#[N:11])[CH:6]=[CH:7][CH:8]=1)[CH3:2].[ClH:13].[NH2:14][C:15]1[C:24]2[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=2)[CH:18]=[CH:17][CH:16]=1>ClCCl>[ClH:13].[C:15]1([NH:14][C:10]([N:9]([C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([CH2:1][CH3:2])[CH:4]=2)[CH3:12])=[NH:11])[C:24]2[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=2)[CH:18]=[CH:17][CH:16]=1

参加物

4

反応物 2

HCID 110941-Naphthalenamine, hydrochloride (1:1)HCID 10103434m-ethylphenyl-N-methylcyanamide

生成物 1

HCID 178436383HCID 178436383、化合物収率 37%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of m-ethylphenyl-N-methylcyanamide (520 mg, 3.25 mmol) and 1-aminonaphthalene hydrochloride (508 mg, 3.25 mmol) was placed in a preheated oil bath at 160° C. for 3 hours and then allowed to cool to room temperature. The resulting solid was taken into dichloromethane and washed with 10% NAOH solution. The organic layer was concentrated and the resulting residue was dissolved in abs. ETOH (2 ml) and treated with dil. HCl. It was concentrated and the solid was twice recrystallized from abs. EtOH-Et2O to give N-(1-naphthyl)-N'-(m-ethylphenyl)-N'-methylguanidine hydrochloride (403 mg, 37%) as off-white needles. mp 223°-25° C.

後処理

  1. washwashed with 10% NAOH solution
  2. concentrationThe organic layer was concentrated
  3. dissolutionthe resulting residue was dissolved in abs
  4. additionETOH (2 ml) and treated with dil. HCl
  5. concentrationIt was concentrated
  6. customthe solid was twice recrystallized from abs

出典と根拠

ORDレコード
ord-37ebb71bf1b94d0992fdb100f4beb874
出典データセット
uspto-grants-1993_11
特許番号
US05262568

関連ノート

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