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1,2-Dichloroethane → HCID 10297462, 화합물

HRID 584129
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HRID 584129 반응식
N(CCCC(OC)=O)=[N+]=[N-].C(C1C=CC(OC)=CC=1)#C.[CH3:21][O:22][C:23]1[CH:28]=[CH:27][C:26]([C:29]2[N:30]=[N:31][N:32]([CH2:34][CH2:35][C:36]([OH:38])=O)[CH:33]=2)=[CH:25][CH:24]=1.[NH2:39][CH2:40][CH2:41][CH2:42][NH:43][C:44]1[C:53]2[C:48](=[CH:49][CH:50]=[CH:51][CH:52]=2)[C:47](=[O:54])[NH:46][N:45]=1.C(Cl)CCl.C(N(CC)CC)C>O1CCOCC1.CN(C=O)C>[CH3:21][O:22][C:23]1[CH:24]=[CH:25][C:26]([C:29]2[N:30]=[N:31][N:32]([CH2:34][CH2:35][C:36]([NH:39][CH2:40][CH2:41][CH2:42][NH:43][C:44]3[C:53]4[C:48](=[CH:49][CH:50]=[CH:51][CH:52]=4)[C:47](=[O:54])[NH:46][N:45]=3)=[O:38])[CH:33]=2)=[CH:27][CH:28]=1
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참가 물질

9

반응물 6

HCID 111,2-DichloroethaneHCID 8471TriethylamineHCID 2510201-Ethynyl-4-methoxybenzeneHCID 111486744-(3-amino-propylamino)-2H-phthalazin-1-oneHCID 11218847HCID 11218847, 화합물HCID 13202491Methyl 4-azidobutanoate

생성물 1

HCID 10297462
HCID 10297462, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 312751,4-Dioxane용매

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온도
175 °C

실험 절차

Methyl 4-azidobutyrate (200 mg, 1.40 mmol) and 1-ethynyl-4-methoxybenzene (277 mg, 210 mmol) were dissolved in dioxane (3 mL) and heated in a microwave reactor for 5 min at 175° C. The reaction mixture was filtered and the filtrate was concentrated under vacuum. Compound 3-[4-(4-methoxy-phenyl)-[1,2,3]triazol-1-yl]-propionic acid methyl ester was treated with aqueous 2M NaOH (5 mL) in THF (3 mL) and stirred at RT for 5 h. The methanol was removed under vacuum and the residue was dissolved in dioxane (5 mL) and treated with concentrated HCl dropwise until a precipitate formed. The resulting acid was collected by filtration and the purity was measured by RPLC (78%). Compound 3-[4-(4-methoxy-phenyl)-[1,2,3]triazol-1-yl]-propionic acid (125 mg, 0.50 mmol) and 4-(3-amino-propylamino)-2H-phthalazin-1-one (100 mg, 0.46 mmol) were dissolved in DMF (2 mL) and treated with EDC (95 mg, 0.50 mmol) and triethylamine (76 mg, 0.75 mmol). 3-[4-(4-Methoxy-phenyl)-[1,2,3]triazol-1-yl]-N-[3-(4-oxo-3,4-dihydro-phthalazin-1-ylamino)-propyl]-propionamide was isolated by preparative RPLC.

후처리

  1. filtrationThe reaction mixture was filtered
  2. concentrationthe filtrate was concentrated under vacuum
  3. additionCompound 3-[4-(4-methoxy-phenyl)-[1,2,3]triazol-1-yl]-propionic acid methyl ester was treated with aqueous 2M NaOH (5 mL) in THF (3 mL)
  4. customThe methanol was removed under vacuum
  5. dissolutionthe residue was dissolved in dioxane (5 mL)
  6. additiontreated with concentrated HCl dropwise until a precipitate
  7. customformed
  8. filtrationThe resulting acid was collected by filtration

출처 및 근거

ORD 기록
ord-172e22f21c0a41459aff890c3b8e969d
출처 데이터셋
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06924284B2

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