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

HRID 556198

반응식

HRID 556198 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

HCID 469280411,8-Bis(chloroacetamido)anthraquinone수율 80%

시약·촉매·용매 2

HCID 1049Pyridine촉매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-9df7afb5faf0465792353d68acb00dbb
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08053583B2

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