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Acetic Acid → 3'-(4-Fluorophenyl)-4-[2-(1,3,5-trimethyl-1H-pyrazol-4-yl)-ethyl]-3,4,5,6-tetrahydro-2H-[1,2']bipyrazine hydrochloride

HRID 220501
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HRID 220501 반응식
[CH3:1][N:2]1[C:6]([CH3:7])=[C:5]([CH2:8][CH:9]=O)[C:4]([CH3:11])=[N:3]1.[F:12][C:13]1[CH:18]=[CH:17][C:16]([C:19]2[C:20]([N:25]3[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]3)=[N:21][CH:22]=[CH:23][N:24]=2)=[CH:15][CH:14]=1.C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(Cl)[Cl:50]>>[ClH:50].[F:12][C:13]1[CH:18]=[CH:17][C:16]([C:19]2[C:20]([N:25]3[CH2:26][CH2:27][N:28]([CH2:9][CH2:8][C:5]4[C:4]([CH3:11])=[N:3][N:2]([CH3:1])[C:6]=4[CH3:7])[CH2:29][CH2:30]3)=[N:21][CH:22]=[CH:23][N:24]=2)=[CH:15][CH:14]=1
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반응물 5

HCID 176Acetic AcidHCID 6344DichloromethaneHCID 5049666Sodium triacetoxyborohydrideHCID 64868769(1,3,5-Trimethyl-1H-pyrazol-4-yl)-acetaldehydeHCID 673669592-(4-Fluorophenyl)-3-(piperazin-1-yl)pyrazine

생성물 1

HCID 68594264
3'-(4-Fluorophenyl)-4-[2-(1,3,5-trimethyl-1H-pyrazol-4-yl)-ethyl]-3,4,5,6-tetrahydro-2H-[1,2']bipyrazine hydrochloride
수율 5%

실험 절차

Combine (1,3,5-trimethyl-1H-pyrazol-4-yl)-acetaldehyde (0.35 g, 2.27 mmol) and 3′-(4-fluorophenyl)-3,4,5,6-tetrahydro-2H-[1,2′]bipyrazinyl (0.71 g, 2.76 mmol) in DCM (10 mL) and stir at room temperature for 10 min. Add glacial acetic acid (0.21 mL, 3.44 mmol) followed by sodium triacetoxyborohydride (0.73 g, 3.44 mmol). Stir at room temperature for 2 hr. Concentrate, dissolve in methanol (5 mL) and load on a 10 g SCX column. Wash with methanol (2×50 mL). Elute with 2 M ammonia in methanol (2×30 mL). Concentrate the eluent and purify (silica gel chromatography, eluting with 45:45:10 hexanes:DCM:ethanol), to give the free base of the title compound (48 mg, 5%). Dissolve the free base (0.041 g, 0.104 mmol) in methanol and add a solution of ammonium chloride (0.006 g, 0.104 mmol) in a minimal volume of methanol. Shake for 18 hr. at room temperature and concentrate to give the title compound (50 mg, 95%). MS (ES): m/z=395 [M+H]+.

후처리

  1. concentrationConcentrate
  2. dissolutiondissolve in methanol (5 mL)
  3. washWash with methanol (2×50 mL)
  4. washElute with 2 M ammonia in methanol (2×30 mL)
  5. concentrationConcentrate the eluent
  6. custompurify
  7. wash(silica gel chromatography, eluting with 45:45:10 hexanes:DCM:ethanol)

출처 및 근거

ORD 기록
ord-da2f02fbfd7d4e56997e4f3c6b9bb55d
출처 데이터셋
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08202873B2

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