Hydrochloric Acid → 5-(6-Isopropyl-1,3-dimethyl-1H-indol-5-yloxy)-pyrimidine-2,4-diamine

HRID 38346

反応式

HRID 38346 の反応式
[CH:1]([C:4]1[CH:12]=[C:11]2[C:7]([C:8]([CH3:14])=[CH:9][N:10]2[CH3:13])=[CH:6][C:5]=1[O:15][C:16](=[CH:19]COC)[C:17]#[N:18])([CH3:3])[CH3:2].C(=O)(O)O.[NH2:27][C:28]([NH2:30])=[NH:29].C[O-].[Na+].Cl>C(O)C.C(OCC)C>[CH:1]([C:4]1[CH:12]=[C:11]2[C:7]([C:8]([CH3:14])=[CH:9][N:10]2[CH3:13])=[CH:6][C:5]=1[O:15][C:16]1[C:17]([NH2:18])=[N:29][C:28]([NH2:30])=[N:27][CH:19]=1)([CH3:2])[CH3:3]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 286947Carbonic acid-guanidine (1:1)HCID 10942334Sodium MethoxideHCID 670534062-(6-Isopropyl-1,3-dimethyl-1H-indol-5-yloxy)-4-methoxy-but-2-enenitrile

生成物 1

HCID 161192135-(6-Isopropyl-1,3-dimethyl-1H-indol-5-yloxy)-pyrimidine-2,4-diamine

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 3283Diethyl Ether溶媒2 回

実験手順

5-(6-Isopropyl-1,3-dimethyl-1H-indol-5-yloxy)-pyrimidine-2,4-diamine was prepared from 2-(6-isopropyl-1,3-dimethyl-1H-indol-5-yloxy)-4-methoxy-but-2-enenitrile by treatment with guanidine carbonate and sodium methoxide using the procedure of step 7 of Example 2 above. This material was dissolved in 2.5 ml absolute ethanol, and 820 ml of 1 N HCl in diethyl ether was added with stirring. Diethyl ether was added slowly until small crystals formed, and the solution was then placed in a −10 C freezer for 18 hours. The solid that had formed was collected by filtration, washed with diethyl ether, and dried under vacuum at 45 C. to give 171 mg. of the hydrochloride salt, Mp: 185.1° C.

後処理

  1. customformed
  2. customThe solid that had formed
  3. filtrationwas collected by filtration
  4. washwashed with diethyl ether
  5. customdried under vacuum at 45 C
  6. customto give 171 mg

出典と根拠

ORDレコード
ord-002d85a37465404faed8fd0a486b2a3b
出典データセット
uspto-grants-2013_09
特許番号
US08524725B2

関連ノート

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