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Hydrochloric Acid → HCID 21106440, 화합물

HRID 1817118
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HRID 1817118 반응식
[C:1]([N:4]1[CH:9]([CH3:10])[CH2:8][N:7]([C:11]2[CH:16]=[C:15]([N:17]3[CH:21]=[N:20][C:19]([NH:22][C:23]4[CH:31]=[CH:30][C:26](C(O)=O)=[CH:25][CH:24]=4)=[N:18]3)[CH:14]=[CH:13][N:12]=2)[CH2:6][CH:5]1[CH3:32])(=[O:3])[CH3:2].CC[N:35](C(C)C)C(C)C.C1C=CC(P(N=[N+]=[N-])(C2C=CC=CC=2)=O)=CC=1.C(O)(C(F)(F)F)=O.Cl>CN1C(=O)CCC1.CO>[NH2:35][C:26]1[CH:30]=[CH:31][C:23]([NH:22][C:19]2[N:20]=[CH:21][N:17]([C:15]3[CH:14]=[CH:13][N:12]=[C:11]([N:7]4[CH2:6][CH:5]([CH3:32])[N:4]([C:1](=[O:3])[CH3:2])[CH:9]([CH3:10])[CH2:8]4)[CH:16]=3)[N:18]=2)=[CH:24][CH:25]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 313Hydrochloric Acid2회HCID 6422Trifluoroacetic acidHCID 81531DiisopropylethylamineHCID 199401P,P-Diphenylphosphinic azideHCID 68419598HCID 68419598, 화합물

생성물 1

HCID 21106440HCID 21106440, 화합물수율 33.6%

시약·촉매·용매

2
HCID 887Methanol용매HCID 13387N-methyl-2-pyrrolidone용매

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온도
25 °C

실험 절차

To a solution of 8 g of 4-{1-[2-(4-Acetyl-3,5-dimethyl-piperazin-1-yl)-pyridin-4-yl]-1H-[1,2,4]triazol-3-ylamino}-benzoic acid (18.3 mMol, 1.00 equiv) in 150 mL of NMP was added 9 mL of Hunig's base followed by 6 g of DPPA (21.8 mMol, 1.19 equiv). The reaction was stirred for 30 min at 25° C. To the reaction mixture was then added 200 mL of TFA and the resulting solution was warmed to 90° C. for 12 hr. After cooling to 25° C., the reaction was quenched with 200 mL of concentrated ammonium hydroxide and concentrated. The resulting oil was triturated with CH2Cl2 and the solid was isolated by filtration. The solid was then dissolved in MeOH (100 mL) and concentrated to 50 mL. The resulting precipitate was isolated and treated with 50 mL of 1 N HCl and concentrated via rotary evaporation. The oil was triturated with ethanol and the resulting solid was removed by filtration. The ethanol solution was concentrated to give 2.5 g of 1-(4-{4-[3-(4-Amino-phenylamino)-[1,2,4]triazol-1-yl]-pyridin-2-yl}-2,6-dimethyl-piperazin-1-yl)-ethanone (6.15 mMol, 33.6% yield) as the HCl salt. 1H NMR (500 MHz, CDCl3) ∂ 8.39 (1H, s), 8.10 (1H, d), 7.22 (2H, d), 7.15 (2H, d), 6.95 (1H, s), 6.92 (2H, m), 6.75 (1H, m), 6.65 (2H, d), 4.15 (2H, m), 3.08 (2H, m), 2.99 (2H, m), 2.10 (3H, s), 1.30 (6H, m) ppm. LC/MS: 0.54 min/407.3 (M+1)

후처리

  1. temperaturethe resulting solution was warmed to 90° C. for 12 hr
  2. temperatureAfter cooling to 25° C.
  3. customthe reaction was quenched with 200 mL of concentrated ammonium hydroxide
  4. concentrationconcentrated
  5. customThe resulting oil was triturated with CH2Cl2
  6. customthe solid was isolated by filtration
  7. concentrationconcentrated to 50 mL
  8. customThe resulting precipitate was isolated
  9. concentrationconcentrated via rotary evaporation
  10. customThe oil was triturated with ethanol
  11. customthe resulting solid was removed by filtration
  12. concentrationThe ethanol solution was concentrated

출처 및 근거

ORD 기록
ord-1607bb6c83e54de3915b45b5326f0038
출처 데이터셋
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07598245B2

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