3-(Dimethylamino)pyrrolidine → HCID 59333673, 화합물

HRID 421342노트

반응식

HRID 421342 반응식
Cl[C:2]1[N:3]([CH2:25][CH:26]2[CH2:28][CH2:27]2)[C:4]2[C:9]([N:10]=1)=[C:8]([N:11]1[CH2:16][CH2:15][O:14][CH2:13][CH2:12]1)[N:7]=[C:6]([C:17]1[C:18]([CH3:24])=[N:19][C:20]([NH2:23])=[N:21][CH:22]=1)[N:5]=2.[CH3:29][N:30]([CH3:36])[CH:31]1[CH2:35][CH2:34][NH:33][CH2:32]1>CN1CCCC1=O>[CH:26]1([CH2:25][N:3]2[C:2]([N:33]3[CH2:34][CH2:35][CH:31]([N:30]([CH3:36])[CH3:29])[CH2:32]3)=[N:10][C:9]3[C:4]2=[N:5][C:6]([C:17]2[C:18]([CH3:24])=[N:19][C:20]([NH2:23])=[N:21][CH:22]=2)=[N:7][C:8]=3[N:11]2[CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)[CH2:28][CH2:27]1

참가 물질

4

반응물 2

HCID 27585193-(Dimethylamino)pyrrolidineHCID 593334985-[8-chloro-9-(cyclopropylmethyl)-6-morpholin-4-yl-9H-purin-2-yl]-4-methylpyrimidin-2-amine

생성물 1

HCID 59333673HCID 59333673, 화합물수율 46%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
120 °C

실험 절차

N-Methylpyrrolidone (1 ml) was added to 5-[8-chloro-9-(cyclopropylmethyl)-6-morpholin-4-yl-9H-purin-2-yl]-4-methylpyrimidin-2-amine (100 mg, 0.25 mmol) and 3-(dimethylamino)pyrolidine (285 mg, 2.49 mmol) and the resulting mixture was stirred at 120° C. for 3.5 hours. The reaction mixture was partitioned with chloroform and saturated brine and the organic layer was washed with saturated brine and dried over magnesium sulfate. The solvent was concentrated under reduced pressure, then methylene chloride-ether was added to the residue, and the precipitate was collected by filtration, washed with ether, and dried under reduced pressure to give the title compound (55 mg, 46%) as a pale orange solid.

후처리

  1. customThe reaction mixture was partitioned with chloroform and saturated brine
  2. washthe organic layer was washed with saturated brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationThe solvent was concentrated under reduced pressure
  5. additionmethylene chloride-ether was added to the residue
  6. filtrationthe precipitate was collected by filtration
  7. washwashed with ether
  8. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-5e5902278c66408f81f866b935670eb0
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08097622B2

반응 노트

불러오는 중…