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1,2-Dichloroethane → HCID 71470591, 화합물

HRID 900166
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HRID 900166 반응식
[C:1]1([C:7]2[C:15]3[C:14]([NH2:16])=[N:13][CH:12]=[N:11][C:10]=3[NH:9][C:8]=2[Si:17]([CH2:22][CH3:23])([CH2:20][CH3:21])[CH2:18][CH3:19])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1.[O:38]1[CH2:42][CH2:41][CH2:40][C@H:39]1[C:43](O)=O.[H-].[Al+3].[Li+].[H-].[H-].[H-]>CN(C1C=CN=CC=1)C.CN(C=O)C.C1COCC1.ClCCl>[C:1]1([C:7]2[C:15]3[C:14]([NH:16][CH2:43][C@@H:39]4[CH2:40][CH2:41][CH2:42][O:38]4)=[N:13][CH:12]=[N:11][C:10]=3[NH:9][C:8]=2[Si:17]([CH2:20][CH3:21])([CH2:22][CH3:23])[CH2:18][CH3:19])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 446666Tetrahydro-2-furoic acid, (-)-HCID 21226445Aluminium lithium hydrideHCID 58603334HCID 58603334, 화합물

생성물 1

HCID 71470591HCID 71470591, 화합물

시약·촉매·용매 4

HCID 14284
4-(Dimethylamino)pyridine
촉매
HCID 6228Dimethylformamide용매
HCID 6344Dichloromethane용매
HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

To a slurry of 4.00 g (12.3 mmol) of 5-phenyl-6-(triethylsilyl)-7-H-pyrrolo[2,3-d]pyrimidin-4-amine, 3.10 g (16.0 mmol) of EDC and 2.50 g (18.5 mmol) of HOBt and catalytic DMAP in 20 ml DMF was added dropwise 1.91 g (14.8 mmol) of (S)-tetrahydro-2-furoic acid at 0° C. The reaction mixture was stirred at 0° C. for 1 h, then was warmed to room temperature and stirred for 30 h. Dichloromethane (500 ml) was added and the mixture was washed with brine (1×), saturated aqueous sodium bicarbonate (1×), and brine (1×). The organic layer was dried over Na2SO4 and filtered. The crude amide was dissolved in 20 ml THF and added to a solution of 700 mg (27.1 mmol) of lithium aluminum hydride in 40 ml THF at 0° C. The slurry was warmed to room temperature and stirred for 1 h, and then to 50° C. and stirred for an additional 2 h. The reaction mixture was cooled to room temperature and poured into ice water. The aqueous material was extracted with ethyl acetate (4×). The combined organic layers were washed with brine (1×), dried over Na2SO4, filtered and purified by chromatography on silica gel (EtOAc:MeOH:Et3N, 9:1:0.1) to give the title compound. 1H-NMR (400 MHz, CDCl3)δ, 0.61 (q, J=7.6 Hz, 6 H), 0.89 (t, J=7.6 Hz, 9 H), 1.48 (m, 1 H), 1.69-1.85 (m, 3 H), 3.59-3.62 (m, 4 H), 3.94 (m, 1 H), 5.03 (s, 1 H), 7.28 (m, 3 H), 7.45 (m, 2 H), 8.33 (s, 1 H), 8.68 (s, 1 H). Mass Spectrum (ESI) m/e=409.1 (M+1).

후처리

  1. temperaturewas warmed to room temperature
  2. stirringstirred for 30 h
  3. washthe mixture was washed with brine (1×), saturated aqueous sodium bicarbonate (1×), and brine (1×)
  4. dry with materialThe organic layer was dried over Na2SO4
  5. filtrationfiltered
  6. dissolutionThe crude amide was dissolved in 20 ml THF
  7. temperatureThe slurry was warmed to room temperature
  8. stirringstirred for 1 h
  9. stirringto 50° C. and stirred for an additional 2 h
  10. temperatureThe reaction mixture was cooled to room temperature
  11. extractionThe aqueous material was extracted with ethyl acetate (4×)
  12. washThe combined organic layers were washed with brine (1×)
  13. dry with materialdried over Na2SO4
  14. filtrationfiltered
  15. custompurified by chromatography on silica gel (EtOAc:MeOH:Et3N, 9:1:0.1)

출처 및 근거

ORD 기록
ord-d8bd987ad3aa46b8a40b3aba8d141d9e
출처 데이터셋
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07358250B2

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