Chloroacetyl chloride → 1,8-Bis(chloroacetamido)anthraquinone

HRID 556198

反応式

HRID 556198 の反応式
[NH2:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][C:12]=3[NH2:17])[C:7](=[O:18])[C:6]=2[CH:5]=[CH:4][CH:3]=1.[Cl:19][CH2:20][C:21](Cl)=[O:22]>CN(C=O)C.N1C=CC=CC=1>[Cl:19][CH2:20][C:21]([NH:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][C:12]=3[NH:17][C:21](=[O:22])[CH2:20][Cl:19])[C:7](=[O:18])[C:6]=2[CH:5]=[CH:4][CH:3]=1)=[O:22]

参加物

5

反応物 2

HCID 6577Chloroacetyl chlorideHCID 85111,8-Diamino-9,10-anthracenedione

生成物 1

HCID 469280411,8-Bis(chloroacetamido)anthraquinone収率 80%

試薬・触媒・溶媒 2

HCID 1049Pyridine触媒HCID 6228Dimethylformamide溶媒

実験手順

Dissolve 1,8-diaminoanthraquinone (0.476 g, 2.0 mmol) in 20 ml DMF. Add pyridine (0.5 ml) as catalyst in an ice bath. Then add chloroacetyl chloride (0.5 ml, 6 mmol) into the solution, remove the ice bath, introduce nitrogen, protect from light, and stir the solution at room temperature for 24 hours. The reacted solution is poured into ice water (50 ml), filtered to get precipitate. At last, the precipitate is recrystallized to get yellow compound 3.

後処理

  1. additionintroduce nitrogen
  2. filtrationfiltered
  3. customto get precipitate
  4. customAt last, the precipitate is recrystallized

出典と根拠

ORDレコード
ord-9df7afb5faf0465792353d68acb00dbb
出典データセット
uspto-grants-2011_11
特許番号
US08053583B2

関連ノート

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