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Sodium hydride → 3-(4-phenoxyphenyl)-1-(tetrahydropyran-4-yl)-1H-pyrazolo[3,4-d]pyrimidin-4-ylamine

HRID 897450
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인쇄 미리보기

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HRID 897450 반응식
[O:1]([C:8]1[CH:13]=[CH:12][C:11]([C:14]2[C:22]3[C:17](=[N:18][CH:19]=[N:20][C:21]=3[NH2:23])[NH:16][N:15]=2)=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Na+].S(C1C=CC(C)=CC=1)(O[CH:30]1[CH2:35][CH2:34][O:33][CH2:32][CH2:31]1)(=O)=O>CC(N(C)C)=O>[O:1]([C:8]1[CH:13]=[CH:12][C:11]([C:14]2[C:22]3[C:17](=[N:18][CH:19]=[N:20][C:21]=3[NH2:23])[N:16]([CH:30]3[CH2:35][CH2:34][O:33][CH2:32][CH2:31]3)[N:15]=2)=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 13961807Tetrahydro-2H-pyran-4-yl 4-methylbenzenesulfonateHCID 178508717HCID 178508717, 화합물2회

생성물 1

HCID 223468363-(4-phenoxyphenyl)-1-(tetrahydropyran-4-yl)-1H-pyrazolo[3,4-d]pyrimidin-4-ylamine수율 18%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

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온도
105 °C

실험 절차

3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-ylamine (Compound 15) (0.97 g) in 33 mL dry dimethylacetamide was stirred under nitrogen while adding 60% sodium hydride (0.22 g). After 30 minutes tetrahydropyran-4-yl tosylate (1.0 g) was added and the mixture heated at 105° C. for 4 hours then 135° C. for 3.5 hours. Evaporation in vacuo and treating with water gave pale brown solid which was collected and washed well with water then dried in air. Flash chromatography in 19:1 ethyl acetate:triethylamine afforded 0.22 g (18%) of 3-(4-phenoxyphenyl)-1-(tetrahydropyran-4-yl)-1H-pyrazolo[3,4-d]pyrimidin-4-ylamine m.p. 187-187.5° C. Calculated for C22H21N5O2 C, 68.2; H, 5.4; N, 18.1; Found C, 68.1; H, 5.5; N, 18.0.

후처리

  1. customEvaporation in vacuo
  2. additiontreating with water
  3. customgave pale brown solid which
  4. customwas collected
  5. washwashed well with water
  6. customthen dried in air

출처 및 근거

ORD 기록
ord-b67f71492f7142dfae31e2c5ab329f89
출처 데이터셋
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06921763B2

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