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Triethylamine → HCID 57593116, 화합물

HRID 1784501
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HRID 1784501 반응식
[C:1]1([C:7]23[CH2:14][CH2:13][C:10]([C:15]([OH:17])=O)([CH2:11][CH2:12]2)[CH2:9][CH2:8]3)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(Cl)(=O)C(Cl)=O.[CH2:24]([O:31][C:32]1[CH:41]=[CH:40][C:35]([C:36]([NH:38][NH2:39])=[O:37])=[C:34]([C:42]([F:45])([F:44])[F:43])[CH:33]=1)[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.C(N(CC)CC)C>C(Cl)Cl.CN(C=O)C>[CH2:24]([O:31][C:32]1[CH:41]=[CH:40][C:35]([C:36]([NH:38][NH:39][C:15]([C:10]23[CH2:9][CH2:8][C:7]([C:1]4[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=4)([CH2:14][CH2:13]2)[CH2:12][CH2:11]3)=[O:17])=[O:37])=[C:34]([C:42]([F:43])([F:44])[F:45])[CH:33]=1)[C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1
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참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 126177784-Phenylbicyclo[2.2.2]octane-1-carboxylic acidHCID 22591719HCID 22591719, 화합물

생성물 1

HCID 57593116HCID 57593116, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide촉매
HCID 6344
Dichloromethane
용매
2회

실험 절차

To a magnetically stirred solution of 4-phenylbicyclo[2.2.2]octane-1-carboxylic acid (8-A) (70 mg, 0.30 mmol) in methylene chloride (1 mL) at room temperature was added 2 M oxalyl chloride in methylene chloride (0.61 mL, 1.22 mmol). Two drops of catalytic DMF were added to catalyze the reaction. The reaction was stirred for 30 min and solvent and reagent removed in vacuo. Methylene chloride (1 mL) was added to the residue, followed by 4-(benzyloxy)-2-(trifluoromethyl)benzoic hydrazide (8-B) (141 mg, 0.46 mmol) and triethylamine (0.07 mL, 0.46 mmol). The reaction was stirred at room temperature overnight to afford intermediate 8-C, N′-[4-(benzyloxy)-2-(trifluoromethyl)benzoyl]-4-phenylbicyclo[2.2.2]octane-1-carbohydrazide, which was not isolated. To the crude product (8-C) were then added 2-chloro-1,3-dimethylimidazolinium chloride (257 mg, 1.52 mmol), more triethylamine (0.42 mL, 3.04 mmol), and methylene chloride (2 mL). The reaction was stirred at room temperature for 4 h. The reaction mixture was then diluted with methylene chloride (30 mL) and washed with water (30 mL) two times and with brine (30 mL) once. The combined aqueous layers were extracted with methylene chloride (25 mL) once. The combined organic layers were dried (MgSO4) and the solvent removed in vacuo. The residue was chromatographed on silica with 10% ethyl acetate in hexanes as eluant to give 2-[4-(benzyloxy)-2-(trifluoromethyl)pheny ]-5-(4-phenylbicyclo[2.2.2]oct-1-yl)-1,3,4-oxadiazole (8-D). MS: m/z 505 (M+1).

후처리

  1. customthe reaction
  2. customsolvent and reagent removed in vacuo
  3. additionMethylene chloride (1 mL) was added to the residue
  4. stirringThe reaction was stirred at room temperature overnight

출처 및 근거

ORD 기록
ord-ff54322d153a4dc4b467848c1630342a
출처 데이터셋
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07504402B2

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