Hydroxyamine hydrochloride → N'-Hydroxy-2-(8-bromonaphthalenyl)ethanimidamide

HRID 330511ノート

反応式

HRID 330511 の反応式
C[O-].[Na+].Cl.[NH2:5][OH:6].[Br:7][C:8]1[CH:9]=[CH:10][CH:11]=[C:12]2[C:17]=1[C:16]([CH2:18][C:19]#[N:20])=[CH:15][CH:14]=[CH:13]2>CO>[OH:6][N:5]=[C:19]([NH2:20])[CH2:18][C:16]1[C:17]2[C:12](=[CH:11][CH:10]=[CH:9][C:8]=2[Br:7])[CH:13]=[CH:14][CH:15]=1

参加物

5

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 10942334Sodium MethoxideHCID 703577032-(8-Bromonaphthalen-1-yl)acetonitrile

生成物 1

HCID 54554816N'-Hydroxy-2-(8-bromonaphthalenyl)ethanimidamide収率 62.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

A mixture of NaOMe (25 wt % in MeOH, 1.6 ml, 6.83 mmol), MeOH (3 mL), and hydroxylamine hydrochloride (0.47 g, 6.83 mmol) was heated for 30 minutes. 8-Bromo-2-naphthalenylacetonitrile (1.12 g, 4.55 mmol) and MeOH (5 mL) were added and heating was continued for 24 hours. The mixture was concentrated, and suspended in H2O (40 mL) and ether (2 mL). The off-white solid was collected by filtration and triturated with ether to give the title compound (790 mg, 62%), m.p. 123°-125° C.

後処理

  1. temperaturewas heated for 30 minutes
  2. temperatureheating
  3. concentrationThe mixture was concentrated
  4. filtrationThe off-white solid was collected by filtration
  5. customtriturated with ether

出典と根拠

ORDレコード
ord-e24a25eaa52f48dfa8a5731afc8f16f9
出典データセット
uspto-grants-1990_01
特許番号
US04897405

反応ノート

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