1-Naphthylamine → HCID 12295945、化合物

HRID 278026ノート

反応式

HRID 278026 の反応式
[N:1]#[C:2]Br.[NH2:4][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH:8]=[CH:7][CH:6]=1>C1(C)C=CC=CC=1>[C:5]1([NH:4][C:2]#[N:1])[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH:8]=[CH:7][CH:6]=1

参加物

4

反応物 2

HCID 86401-NaphthylamineHCID 10476Cyanogen Bromide

生成物 1

HCID 12295945HCID 12295945、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Cyanogen bromide (4.4 gm, 41.9 mmol) was added in portions to the stirred and ice-bath cooled solution of 1-aminonaphthalene (10.0 gm, 69.8 mmol) in toluene (100 mL). After 0.5 hour, the cooling bath was removed the reaction mixture was stirred at room temperature for 12 hours. The precipitate was filtered and the solid was triturated with water (150 mL) for 0.5 hour. The resulted solid was filtered and washed with water (4×20 mL) and the solid was dried in vacuum oven at 40° C. This material (4.6 gm) was used as such without any further purification.

後処理

  1. customthe cooling bath was removed the reaction mixture
  2. stirringwas stirred at room temperature for 12 hours
  3. filtrationThe precipitate was filtered
  4. customthe solid was triturated with water (150 mL) for 0.5 hour
  5. filtrationThe resulted solid was filtered
  6. washwashed with water (4×20 mL)
  7. customthe solid was dried in vacuum oven at 40° C
  8. customsuch without any further purification

出典と根拠

ORDレコード
ord-d4901e41c2b2428b94ea0144e652eff6
出典データセット
uspto-grants-2002_03
特許番号
US06358993B1

反応ノート

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