Ethanol → HCID 69588754、化合物

HRID 890251

反応式

HRID 890251 の反応式
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([N:12]3[C:17]([Cl:18])=[C:16]([S:19][CH3:20])[C:15](Cl)=[N:14][CH:13]3[NH2:22])[CH:10]=2)[N:5]=C(C)[CH:3]=1.[NH2:24][C:25]1[C:34]2[C:29](=[CH:30][CH:31]=[C:32]([NH2:35])[CH:33]=2)[N:28]=[C:27]([CH3:36])[CH:26]=1.[CH2:37](O)[CH3:38]>>[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([N:12]3[C:17]([Cl:18])=[C:16]([S:19][CH3:20])[CH:15]([NH2:14])[N:35]([C:32]4[CH:33]=[C:34]5[C:29](=[CH:30][CH:31]=4)[N:28]=[C:27]([CH3:36])[CH:26]=[C:25]5[NH2:24])[CH:13]3[NH2:22])[CH:10]=2)[N:5]=[C:37]([CH3:38])[CH:3]=1

参加物

4

反応物 3

HCID 702EthanolHCID 2239952-Methylquinoline-4,6-diamineHCID 22250299HCID 22250299、化合物

生成物 1

HCID 69588754HCID 69588754、化合物

実験手順

A mixture of 43 mg of N-(4-amino-2-methyl-6-quinolyl)-2-amino-4,6-dichloro-5-methylsulfanylpyrimidine and 55 mg of 4,6-diamino-2-methylquinoline in 5 mL of ethanol is heated under reflux for about 3 hours, left at a temperature in the region of 20° C. for about 16 hours and then filtered. The filtrate is concentrated under reduced pressure (2.7 kPa) at a temperature in the region of 40° C., and then the residue obtained is purified by HPLC (column: C18 Waters, 5 M, 50×19 mm; eluent: elution gradient water-acetonitrile-TFA (0.07%) from 95-5 to 5-95 over 30 minutes). The fractions containing the desired product are combined and concentrated to dryness under reduced pressure (2.7 kPa) at a temperature in the region of 40° C. to obtain 12 mg of N,N′-bis(4-amino-2-methyl-6-quinolyl)-2,4-diamino-6-chloro-5-methylsulfanyl-pyrimidine in the form of a beige colored solid.

後処理

  1. temperatureis heated
  2. temperatureunder reflux for about 3 hours
  3. filtrationfiltered
  4. concentrationThe filtrate is concentrated under reduced pressure (2.7 kPa) at a temperature in the region of 40° C.
  5. customthe residue obtained
  6. customis purified by HPLC (column
  7. washeluent: elution gradient water-acetonitrile-TFA (0.07%) from 95-5 to 5-95 over 30 minutes)
  8. additionThe fractions containing the desired product
  9. concentrationconcentrated to dryness under reduced pressure (2.7 kPa) at a temperature in the region of 40° C.

出典と根拠

ORDレコード
ord-9bf56a2bfb094f739b344600036807a4
出典データセット
uspto-grants-2006_02
特許番号
US06995175B2

関連ノート

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