Potassium Carbonate → HCID 22341120、化合物

HRID 584683ノート

反応式

HRID 584683 の反応式
Cl[C:2]1[C:11]([CH2:12][CH2:13][CH2:14]Cl)=[N:10][C:9]2[C:4](=[CH:5][C:6]([Cl:17])=[C:7]([Cl:16])[CH:8]=2)[N:3]=1.[SH-:18].[Na+].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:16][C:7]1[CH:8]=[C:9]2[C:4](=[CH:5][C:6]=1[Cl:17])[N:3]=[C:2]1[C:11]([CH2:12][CH2:13][CH2:14][S:18]1)=[N:10]2

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 28015Sodium hydrosulfideHCID 22341136HCID 22341136、化合物

生成物 1

HCID 22341120HCID 22341120、化合物収率 100%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 2,6,7-trichloro-3-(3-chloropropyl)quinoxaline (0.15 g, 0.48 mmol) in dry DMF (50 ml) were added sodium hydrosulfide (0.11 g, 1.44 mmol) and potassium carbonate (0.20 g, 1.45 mmol). The reaction mixture was stirred for 4 days at room temperature. The solvent was evaporated in vacuo, followed by the addition of water. The resulting mixture was extracted with dichloromethane (3×). The combined organic layers were dried over anhydrous sodium sulfate, filtered and evaporated in vacuo to yield 6,7-dichloro-3,4-dihydro-2H-1-thia-9,10-diaza-anthracene (>100%) as a solid.

後処理

  1. customThe solvent was evaporated in vacuo
  2. additionfollowed by the addition of water
  3. extractionThe resulting mixture was extracted with dichloromethane (3×)
  4. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. customevaporated in vacuo

出典と根拠

ORDレコード
ord-d5b5f3b0e424436f94b7bfabd800e215
出典データセット
uspto-grants-2005_08
特許番号
US06927214B1

反応ノート

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