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Toluene → HCID 86698714, 화합물

HRID 338371
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HRID 338371 반응식
[Cl:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6]([C:11]([O:13][CH3:14])=[O:12])=[CH:7][NH:8]2)=[CH:4][C:3]=1B1OCC(C)(C)CO1.Cl.Br[C:25]1[CH:30]=[CH:29][C:28]([CH:31]2[CH2:34][CH2:33][NH:32]2)=[CH:27][CH:26]=1.C(=O)([O-])[O-].[K+].[K+].C1(C)C=CC=CC=1>C(OCC)(=O)C.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].ClCCl.C(O)C>[NH:32]1[CH2:33][CH2:34][CH:31]1[C:28]1[CH:29]=[CH:30][C:25]([C:3]2[CH:4]=[C:5]3[C:9](=[CH:10][C:2]=2[Cl:1])[NH:8][CH:7]=[C:6]3[C:11]([O:13][CH3:14])=[O:12])=[CH:26][CH:27]=1
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참가 물질

8

반응물 4

HCID 1140TolueneHCID 11430Potassium CarbonateHCID 86698665methyl 6-chloro-5-(5,5-dimethyl-1,3,2-dioxaborinan-2-yl)-1H-indole-3-carboxylateHCID 866987152-(4-bromophenyl)azetidine hydrochloride

생성물 1

HCID 86698714HCID 86698714, 화합물수율 379.6%

시약·촉매·용매 3

HCID 178418807
HCID 178418807, 화합물
촉매
HCID 702Ethanol용매
HCID 8857Ethyl Acetate용매

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온도
100 °C

실험 절차

A mixture of methyl 6-Chloro-5-(5,5-dimethyl-[1,3,2]dioxaborinan-2-yl)-1H-indole-3-carboxylate (50 mg, 0.16 mmol), 2-(4-bromophenyl)azetidine hydrochloride (400 mg, 1.24 mmol), 2M aqueous potassium carbonate (3.11 mL, 6.22 mmol), toluene (9 mL), and ethanol (3 mL) was sparged with nitrogen for 10 minutes, then treated with [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) dichloromethane adduct (46 mg, 0.056 mmol). The reaction mixture was heated to 100° C. and stirred. After 2 hours the reaction was cooled to room temperature, diluted with ethyl acetate, washed with water and saturated brine, dried over magnesium sulfate, filtered and concentrated in vacuo to afford a yellow oil, which was purified by flash chromatography (40 g silica, 0-40% methanol/ethyl acetate (1% TEA modifier), 24 column volumes). Product fractions were combined and concentrated in vacuo to afford the title compound as a yellow solid (207 mg, 49% yield). MS (ES+) 341.2 (M+H)+; 1H NMR (500 MHz, CD3OD) δ 7.98 (d, J=3.90 Hz, 2H), 7.56 (s, 1H), 7.41 (s, 4H), 5.02 (t, J=8.17 Hz, 1H), 3.84 (s, 3H), 3.68-3.79 (m, 1H), 3.34-3.45 (m, 1H), 2.47-2.66 (m, 2H).

후처리

  1. customwas sparged with nitrogen for 10 minutes
  2. temperatureAfter 2 hours the reaction was cooled to room temperature
  3. washwashed with water and saturated brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customto afford a yellow oil, which
  8. customwas purified by flash chromatography (40 g silica, 0-40% methanol/ethyl acetate (1% TEA modifier), 24 column volumes)
  9. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-44659f953fa342f1a5b8847e7e59f272
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08889730B2

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