2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → HCID 178456711, 화합물

HRID 979315노트

반응식

HRID 979315 반응식
[OH:1][C:2]1[CH:15]=[C:14]2[C:5]([NH:6][C:7]3[C:12]([S:13]2(=[O:17])=[O:16])=[CH:11][CH:10]=[CH:9][CH:8]=3)=[C:4]2[CH:18]=[CH:19][CH:20]=[CH:21][C:3]=12.ClC1C(=O)[C:25](C#N)=[C:26]([C:31]#[N:32])C(=O)C=1Cl.C(N)CC>C1COCC1>[CH2:31]([NH:32][C:15]1[C:2](=[O:1])[C:3]2[CH:21]=[CH:20][CH:19]=[CH:18][C:4]=2[C:5]2[C:14]=1[S:13](=[O:17])(=[O:16])[C:12]1[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=1)[N:6]=2)[CH2:26][CH3:25]

참가 물질

5

반응물 3

HCID 67752,3-Dichloro-5,6-dicyano-1,4-benzoquinoneHCID 7852PropylamineHCID 137124805-Hydroxy-12H-benzo[a]phenothiazine-7,7-dioxide

생성물 1

HCID 178456711HCID 178456711, 화합물수율 62.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a suspension of 5-hydroxy-12H-benzo[a]phenothiazine-7,7-dioxide (594 mg) in THF (10 ml) was added 2,3-dichloro 5,6-dicyano-1,4-benzoquinone (1.021 gram). The mixture was stirred at room temperature for 2 minutes, then there was added n-propyl amine (0.2 ml). The stirring was continued for 0.5 hour, then the mixture was evaporated to dryness. To the residue was added 50 ml dichloromethane and the mixture was stirred for 15 minutes and filtered. The filtrate was evaporated to dryness and the residue crystallized from a mixture of toluene and hexane to afford the title compound (442 mg) as a red-brown crystalline solid, m.p. 149°-151° C. (dec.).

후처리

  1. waitThe stirring was continued for 0.5 hour
  2. customthe mixture was evaporated to dryness
  3. additionTo the residue was added 50 ml dichloromethane
  4. stirringthe mixture was stirred for 15 minutes
  5. filtrationfiltered
  6. customThe filtrate was evaporated to dryness
  7. customthe residue crystallized from a mixture of toluene and hexane

출처 및 근거

ORD 기록
ord-4c457c88b89346088d00c22d419648ef
출처 데이터셋
uspto-grants-1987_05
특허 번호
US04667032

반응 노트

불러오는 중…