2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → HCID 178456711、化合物

HRID 979315ノート

反応式

HRID 979315 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 178456711HCID 178456711、化合物収率 62.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-4c457c88b89346088d00c22d419648ef
出典データセット
uspto-grants-1987_05
特許番号
US04667032

反応ノート

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