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4-Methoxybenzoic Acid → HCID 10252289, 화합물

HRID 567105
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HRID 567105 반응식
[CH3:1][O:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]([OH:9])=O)=[CH:5][CH:4]=1.ON1C2C=CC=CC=2N=N1.Cl.CN(C)CCCN=C=NCC.[F:34][C:35]([F:53])([F:52])[O:36][C:37]1[CH:42]=[CH:41][C:40]([CH:43]2[C:48]3[CH:49]=[CH:50][S:51][C:47]=3[CH2:46][CH2:45][NH:44]2)=[CH:39][CH:38]=1.C(N(CC)C(C)C)(C)C>CN(C)C=O.O>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([C:7]([N:44]2[CH2:45][CH2:46][C:47]3[S:51][CH:50]=[CH:49][C:48]=3[CH:43]2[C:40]2[CH:39]=[CH:38][C:37]([O:36][C:35]([F:34])([F:53])[F:52])=[CH:42][CH:41]=2)=[O:9])=[CH:10][CH:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 74784-Methoxybenzoic AcidHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 2777349HCID 2777349, 화합물

생성물 1

HCID 10252289HCID 10252289, 화합물수율 117%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

4-Methoxybenzoic acid (0.64 g, 4.2 mmol) was dissolved in N,N-dimethylformamide (25 ml) and 1-hydroxybenzotriazole (0.71 g, 5 mmol) was added followed by N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (0.96 g, 5 mmol). The resulting mixture was stirred at room temperature for 30 minutes. 4-(4-Trifluoromethoxyphenyl)-4,5,6,7-tetrahydro-thieno[3,2-c]pyridine (1.5 g, 5 mmol) followed by N,N-diisopropylethylamine (1.4 ml, 8.4 mmol) were added and the resulting mixture was stirred at room temperature for 16 hours. Water (10 ml) was added and the mixture was extracted with diethyl ether (3×20 ml). The combined organic extracts were washed with saturated aqueous ammonium chloride (20 ml), dried over MgSO4 and concentrated in vacuo. The residue was purified by column chromatography over silica gel eluting with a mixture of ethyl acetate and heptane (1:2). The pure fractions were pooled and concentrated in vacuo. The residue was crystallised from a mixture of methyl tert-butyl ether and heptane to afford 2.13 g (98%) of the title compound.

후처리

  1. additionwere added
  2. stirringthe resulting mixture was stirred at room temperature for 16 hours
  3. extractionthe mixture was extracted with diethyl ether (3×20 ml)
  4. washThe combined organic extracts were washed with saturated aqueous ammonium chloride (20 ml)
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by column chromatography over silica gel eluting with a mixture of ethyl acetate and heptane (1:2)
  8. concentrationconcentrated in vacuo
  9. customThe residue was crystallised from a mixture of methyl tert-butyl ether and heptane

출처 및 근거

ORD 기록
ord-9efe03e4df4c450e9631c7f33b973282
출처 데이터셋
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06177443B1

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