1,8-Diamino-9,10-anthracenedione → 1,8-Bis(3-chloropropionamido)anthraquinone

HRID 556205

反応式

HRID 556205 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][CH2:21][C:22](Cl)=[O:23]>CN(C)C=O.N1C=CC=CC=1>[Cl:19][CH2:20][CH2:21][C:22]([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:22](=[O:23])[CH2:21][CH2:20][Cl:19])[C:7](=[O:18])[C:6]=2[CH:5]=[CH:4][CH:3]=1)=[O:23]

参加物

5

反応物 2

HCID 85111,8-Diamino-9,10-anthracenedioneHCID 693643-Chloropropionyl chloride

生成物 1

HCID 107407551,8-Bis(3-chloropropionamido)anthraquinone収率 58%

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 mmol) in N,N-dimethylformamide (20 ml). Add pyridine (0.5 ml) as catalyst in an ice bath and then add 3-chloropropioyl chloride (0.6 ml, 6 mmol). Remove the ice bath, introduce nitrogen, protect from light, and stir the solution at room temperature for one day. The reacted mixture is poured into ice water and filtered to get precipitate. The precipitate is recrystallized from ethanol to obtain orange compound 4.

後処理

  1. customRemove the ice bath
  2. additionintroduce nitrogen
  3. additionThe reacted mixture is poured into ice water
  4. filtrationfiltered
  5. customto get precipitate
  6. customThe precipitate is recrystallized from ethanol

出典と根拠

ORDレコード
ord-7128a3e17df04099b9867a2f2d98eb81
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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