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Hydroxylamine → HCID 11705851, 화합물

HRID 1723816
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HRID 1723816 반응식
[CH3:1][S:2]([N:5]1[CH2:10][CH2:9][N:8]([C:11]2[CH:16]=[CH:15][C:14]([O:17][CH2:18][C:19]([F:22])([F:21])[F:20])=[CH:13][N:12]=2)[CH2:7][CH2:6]1)(=[O:4])=[O:3].[Li+].C[Si]([N-:28][Si](C)(C)C)(C)C.P(Cl)(OCC)(OCC)=O.[N:42]1[CH:47]=[CH:46][CH:45]=[CH:44][C:43]=1[CH2:48][CH2:49]C=O.[NH2:52][OH:53]>C1COCC1>[OH:53][NH:52][CH:49]([CH2:1][S:2]([N:5]1[CH2:10][CH2:9][N:8]([C:11]2[CH:16]=[CH:15][C:14]([O:17][CH2:18][C:19]([F:22])([F:20])[F:21])=[CH:13][N:12]=2)[CH2:7][CH2:6]1)(=[O:4])=[O:3])[CH2:48][CH2:43][C:42]1[N:47]=[CH:46][CH:45]=[CH:44][N:28]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 787HydroxylamineHCID 13139Diethyl chlorophosphateHCID 2733832Lithium hexamethyldisilazaneHCID 114007983-(Pyridin-2-YL)propanalHCID 575592331-(Methanesulfonyl)-4-[5-(2,2,2-trifluoroethoxy)pyridin-2-yl]piperazine

생성물 1

HCID 11705851HCID 11705851, 화합물수율 95%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

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온도
0 °C

실험 절차

To a stirred suspension 1-(methylsulfonyl)-4-[5-(2,2,2-trifluoroethoxy)pyridin-2-yl]piperazine (23 g, 67.8 mmol, prepared as above) in THF (450 mL) at −65° C., was added drop wise a solution of LiHMDS in THF (149 mL, 1.0M solution, 149 mmol). Stirred for 30 minutes. Added diethyl chlorophosphate (11.3 mL, 78 mmol) and stirred for 1 hour. The solution was treated drop wise with a solution of 3-(2-pyridinyl)propaldehyde (12 g, 88.1 mmol) in THF (290 mL) and then allowed to warm to 0° C. over 3 hours before being quenched with a solution of hydroxylamine (41 mL, 50% aqueous solution in water, 680 mmol). The reaction was stirred for 16 hours at RT. The reaction washed with sat. NH4Cl (250 mL) back-extracting with ethyl acetate (250 mL). The combined organic extracts were then dried (brine and MgSO4), filtered and concentrated in vacuo. The residue was then triturated with ether for 1 hour, filtered and dried to give 2-[3-(hydroxyamino)-4-({4-[5-(2,2,2-trifluoroethoxy)pyridin-2-yl]piperazin-1-yl}sulfonyl)butyl]pyrimidine (31.5 g, 64.3 mmol, 95%).

후처리

  1. stirringThe reaction was stirred for 16 hours at RT
  2. washThe reaction washed with sat. NH4Cl (250 mL)
  3. extractionback-extracting with ethyl acetate (250 mL)
  4. dry with materialThe combined organic extracts were then dried (brine and MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue was then triturated with ether for 1 hour
  8. filtrationfiltered
  9. customdried

출처 및 근거

ORD 기록
ord-dccfc69233404a4db435fef5cd57141b
출처 데이터셋
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07485644B2

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