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

HRID 38346

반응식

HRID 38346 반응식
[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]

참가 물질

7

반응물 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

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매HCID 3283Diethyl Ether용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-002d85a37465404faed8fd0a486b2a3b
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524725B2

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