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Ammonia methanol → 5-iodo-7-((2-(trimethylsilyl)ethoxy)methyl)-7H-pyrrolo[2,3-d]pyrimidin-4-amine

HRID 336164
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HRID 336164 반응식
CO.[NH3:3].Cl[C:5]1[C:6]2[C:13]([I:14])=[CH:12][N:11]([CH2:15][O:16][CH2:17][CH2:18][Si:19]([CH3:22])([CH3:21])[CH3:20])[C:7]=2[N:8]=[CH:9][N:10]=1>CO.O>[I:14][C:13]1[C:6]2[C:5]([NH2:3])=[N:10][CH:9]=[N:8][C:7]=2[N:11]([CH2:15][O:16][CH2:17][CH2:18][Si:19]([CH3:22])([CH3:21])[CH3:20])[CH:12]=1
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참가 물질

5

반응물 2

HCID 21705897Ammonia methanolHCID 867069334-chloro-5-iodo-7-((2-(trimethylsilyl)ethoxy)methyl)-7H-pyrrolo[2,3-d]pyrimidine

생성물 1

HCID 685729975-iodo-7-((2-(trimethylsilyl)ethoxy)methyl)-7H-pyrrolo[2,3-d]pyrimidin-4-amine

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

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온도
120 °C

실험 절차

An 8 N ammonia methanol solution (120 ml) was added to the 4-chloro-5-iodo-7-((2-(trimethylsilyl)ethoxy)methyl)-7H-pyrrolo[2,3-d]pyrimidine (20.0 g) obtained in Step 1, and the mixture was stirred in a microwave reactor at 120° C. for 1 hour. After being cooled, the reaction mixture was diluted with methanol (65 ml) and water (185 ml). The resulting precipitate was collected by filtration, washed with water, and dried under reduced pressure to obtain the title compound (15.2 g) as a white solid.

후처리

  1. temperatureAfter being cooled
  2. filtrationThe resulting precipitate was collected by filtration
  3. washwashed with water
  4. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-a80e89840ffd4f02abce38cd30bb1b8d
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08889666B2

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