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Toluene → HCID 118062866, 화합물

HRID 920759
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HRID 920759 반응식
CC1CC([C:6]([OH:8])=O)C1.C1C=CC(P([N:23]=[N+]=[N-])(C2C=CC=CC=2)=O)=CC=1.[Cl:26][C:27]1[CH:28]=[C:29]([C:34]2[C:42]([C:43]([NH2:45])=[O:44])=[C:37]3[CH2:38][NH:39][CH2:40][CH2:41][N:36]3[N:35]=2)[CH:30]=[CH:31][C:32]=1[F:33].[C:46]1([CH3:52])[CH:51]=[CH:50][CH:49]=CC=1>C1COCC1>[Cl:26][C:27]1[CH:28]=[C:29]([C:34]2[C:42]([C:43]([NH2:45])=[O:44])=[C:37]3[CH2:38][N:39]([C:6]([NH:23][CH:46]4[CH2:51][CH:50]([CH3:49])[CH2:52]4)=[O:8])[CH2:40][CH2:41][N:36]3[N:35]=2)[CH:30]=[CH:31][C:32]=1[F:33]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

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HCID 1140TolueneHCID 199401P,P-Diphenylphosphinic azideHCID 3044406Cyclobutanecarboxylic acid, 3-methyl-HCID 1180616272-(3-Chloro-4-fluorophenyl)-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrazine-3-carboxamide

생성물 1

HCID 118062866HCID 118062866, 화합물

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

실험 절차

A solution of Intermediate 246A (77 mg, 0.679 mmol), TEA (0.142 mL, 1.018 mmol) and DPPA (0.146 mL, 0.679 mmol) in toluene (5 mL) was stirred at 90° C. for 2 h. The reaction mixture was cooled to RT and to it was added a solution of Intermediate 185B (100 mg, 0.339 mmol) in THF (1 mL) and stirred at RT for 4 h. The reaction mixture was quenched with water and the aqueous layer was extracted with ethyl acetate (3×5 mL) The combined organic layer was washed with an aqueous solution of 10% aq. NaHCO3, water, dried over Na2SO4, filtered and the filtrate concentrated to afford the crude product as an off-white solid. The crude material was purified by preparative TLC. The crude material was loaded on a 0.5 mm silica gel plate and developed using 6% MeOH in CHCl3. The band containing the desired product was separated and extracted into 10% MeOH in DCM, filtered and the filtrate concentrated to afford a mixture cis and trans isomers as an off-white solid. The individual isomers were separated using preparative chiral SFC purification.

후처리

  1. customThe reaction mixture was quenched with water
  2. extractionthe aqueous layer was extracted with ethyl acetate (3×5 mL) The combined organic layer
  3. washwas washed with an aqueous solution of 10% aq. NaHCO3, water
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationthe filtrate concentrated

출처 및 근거

ORD 기록
ord-47b0caac386246ccb551c2359d30fe27
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09273058B2

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