Triethylamine → 4-[2-(2-Aminopyrimidin-5-yl)-9-isobutyl-6-morpholin-4-yl-9H-purin-8-yl]-N,N-dimethylpiperazine-1-carboxamide

HRID 421352

반응식

HRID 421352 반응식
C(N(CC)CC)C.[CH2:8]([N:12]1[C:20]([N:21]2[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]2)=[N:19][C:18]2[C:13]1=[N:14][C:15]([C:33]1[CH:34]=[N:35][C:36]([NH2:39])=[N:37][CH:38]=1)=[N:16][C:17]=2[N:27]1[CH2:32][CH2:31][O:30][CH2:29][CH2:28]1)[CH:9]([CH3:11])[CH3:10].[CH3:40][N:41]1[CH2:45]CC[C:42]1=[O:46]>>[NH2:39][C:36]1[N:37]=[CH:38][C:33]([C:15]2[N:14]=[C:13]3[C:18]([N:19]=[C:20]([N:21]4[CH2:26][CH2:25][N:24]([C:42]([N:41]([CH3:45])[CH3:40])=[O:46])[CH2:23][CH2:22]4)[N:12]3[CH2:8][CH:9]([CH3:11])[CH3:10])=[C:17]([N:27]3[CH2:32][CH2:31][O:30][CH2:29][CH2:28]3)[N:16]=2)=[CH:34][N:35]=1

참가 물질

4

반응물 3

HCID 8471TriethylamineHCID 13387N-methyl-2-pyrrolidoneHCID 593335015-(9-Isobutyl-6-morpholino-8-(piperazin-1-yl)-9H-purin-2-yl)pyrimidin-2-amine

생성물 1

HCID 593336134-[2-(2-Aminopyrimidin-5-yl)-9-isobutyl-6-morpholin-4-yl-9H-purin-8-yl]-N,N-dimethylpiperazine-1-carboxamide수율 43%

실험 절차

Triethylamine (64 μl) and 2-acetamide-4-dimethylcarbamoyl chloride (35 μl) were added to an N-methylpyrrolidone solution (1 ml) of 5-(9-isobutyl-6-morpholin-4-yl-8-piperazin-1-yl-9H-purin-2-yl)pyrimidin-2-ylamine (100 mg) and the resulting mixture was stirred for 24 hours. The reaction mixture was partitioned with ethyl acetate and water, the insoluble solid was collected by filtration, and then the organic layer of the filtrate was dried over magnesium sulfate. The solvent was evaporated under reduced pressure, the residue was combined with the solid separately collected by filtration followed by the addition of dimethyl sulfoxide (3 ml) and water (3 ml), the resulting mixture was stirred, and the insoluble matter was collected by filtration, washed with water, and dried to give the title compound (50 mg, 43%) as a pale yellow solid.

후처리

  1. customThe reaction mixture was partitioned with ethyl acetate and water
  2. filtrationthe insoluble solid was collected by filtration
  3. dry with materialthe organic layer of the filtrate was dried over magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. filtrationseparately collected by filtration
  6. additionfollowed by the addition of dimethyl sulfoxide (3 ml) and water (3 ml)
  7. stirringthe resulting mixture was stirred
  8. filtrationthe insoluble matter was collected by filtration
  9. washwashed with water
  10. customdried

출처 및 근거

ORD 기록
ord-afd9331e856a453cab1609a14fad63fd
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08097622B2

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