Dimethylformamide → HCID 21072031, compound

HRID 1372794Notes

Reaction equation

HRID 1372794 reaction equation
[OH:1][CH2:2][CH2:3][NH:4][C:5]1[C:18]2[C:17](=[O:19])[C:16]3[C:11](=[C:12]([NH:21][CH2:22][CH2:23][OH:24])[CH:13]=[C:14](Br)[CH:15]=3)[C:10](=[O:25])[C:9]=2[CH:8]=[C:7](Br)[CH:6]=1.CN(C)C=O.[C:32]1([S-:38])[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1.[Na+]>CO>[OH:1][CH2:2][CH2:3][NH:4][C:5]1[C:18]2[C:17](=[O:19])[C:16]3[C:11](=[C:12]([NH:21][CH2:22][CH2:23][OH:24])[CH:13]=[C:14]([S:38][C:32]4[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=4)[CH:15]=3)[C:10](=[O:25])[C:9]=2[CH:8]=[C:7]([S:38][C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[CH:6]=1

Participants

5

Reactant 3

HCID 6228DimethylformamideHCID 4110039Sodium benzenethiolateHCID 21072032HCID 21072032, compound

Product 1

HCID 21072031HCID 21072031, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Conditions

Temperature
120 °C

Procedure

24 g of 1,5-bis(2-hydroxyethylamino)-3,7-dibromoanthraquinone are introduced at RT into 100 ml of dimethylformamide (DMF). After the addition of 16.3 g of sodium thiophenolate, the mixture is heated to 120° C. and maintained at that temperature for one hour. After cooling the mixture to RT, 100 ml of methanol are added thereto. The precipitate is filtered off, washed with a methanol/water mixture (1:1) and dried in vacuo.

Workup

  1. temperaturemaintained at that temperature for one hour
  2. temperatureAfter cooling the mixture to RT
  3. filtrationThe precipitate is filtered off
  4. washwashed with a methanol/water mixture (1:1)
  5. customdried in vacuo

Sources & evidence

ORD record
ord-31ae0a7575c74bbebcad34c4035dd50b
Source dataset
uspto-grants-2007_01
Patent number
US07160335B2

Reaction notes

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