4-Bromo-1-naphthylamine → 1-Bromo-4-isothiocyanatonaphthalene

HRID 1042638

反応式

HRID 1042638 の反応式
[Br:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([NH2:12])=[CH:4][CH:3]=1.N1([C:18](N2C=CN=C2)=[S:19])C=CN=C1>ClCCl>[Br:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([N:12]=[C:18]=[S:19])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 753034-Bromo-1-naphthylamineHCID 802641,1'-Thiocarbonyldiimidazole

生成物 1

HCID 4593621-Bromo-4-isothiocyanatonaphthalene

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 1-bromo-4-aminonapthalene (2.6 g, 12 mmol) in dichloromethane (45 mL) was added di(1H-imidazol-1-yl)methanethione (2.1 g, 12 mmol). The reaction was allowed to stir for 16 h, at which point the reaction was concentrated to give a gray solid. The solid was slurried in 50% EtOAc/hexanes and filtered through a pad of silica gel, rinsing with 400 mL 50% EtOAc/hexanes. The solution was concentrated to give 1-bromo-4-isothiocyanatonaphthalene as a gray solid, which was used without further purification.

後処理

  1. concentrationwas concentrated
  2. customto give a gray solid
  3. filtrationfiltered through a pad of silica gel
  4. washrinsing with 400 mL 50% EtOAc/hexanes
  5. concentrationThe solution was concentrated

出典と根拠

ORDレコード
ord-041c880270f0457e9dbb63395c327f26
出典データセット
uspto-grants-2013_10
特許番号
US08557996B2

関連ノート

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