1-Naphthalenamine, hydrochloride (1:1) → HCID 178436383, 화합물

HRID 964164

반응식

HRID 964164 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 178436383HCID 178436383, 화합물수율 37%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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 pre-heated 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'-methyl-guanidine hydrochloride (403 mg, 37%) as off-white needles. mp 223°-25° C.

후처리

  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

출처 및 근거

ORD 기록
ord-3cd5715e2e634fa5a674200120003d55
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05767162

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