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Hydrochloric Acid → HCID 22221600, 화합물

HRID 1794528
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HRID 1794528 반응식
Br[C:2]1[CH:7]=[C:6]([OH:8])[CH:5]=[CH:4][C:3]=1[C:9]1[O:10][C:11]2[CH:17]=[CH:16][C:15]([OH:18])=[CH:14][C:12]=2[CH:13]=1.[C:19]1(B(O)O)[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.Cl.[CH3:29][CH2:30][OH:31]>C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH2:30]([O:31][C:5]1[C:6]([OH:8])=[CH:7][C:2]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[C:3]([C:9]2[O:10][C:11]3[CH:17]=[CH:16][C:15]([OH:18])=[CH:14][C:12]=3[CH:13]=2)[CH:4]=1)[C:29]1[CH:6]=[CH:7][CH:2]=[CH:3][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 66827Phenylboronic AcidHCID 10236546HCID 10236546, 화합물

생성물 1

HCID 22221600HCID 22221600, 화합물

시약·촉매·용매 1

HCID 178418397HCID 178418397, 화합물촉매

실험 절차

Compound 102 (0.23 g, 7.9 mmol) in a solution consisting of Tol/EtOH/2M Na2CO3 aq (15 mL/2 mL/15 mL) was treated with 4-benzloxy phenylboronic acid (0.12 g, 1.0 mmol) and cat Pd(PPh3)4 and heated to reflux until TLC analysis indicated complete reaction. The reaction mixture was treated with 2 N HCl aq and extracted with EtOAc. The EtOAc layer was washed with saturated NaHCO3 aq, brine and dried over MgSO4. After filtration, the residue was chromatographed on silica gel (1:4 EtOAc/hexanes) to yield the desired product as an orange solid. The orange solid thus obtained was triturated with CH2Cl2 to yield the pdt (2.4 g) as a white solid: Mp=186–187° C.; 1H NMR (DMSO-d6) δ 9.90 (br s, 1 H), 9.05 (br s, 1 H), 7.65 (d, 1 H, J=8.5 Hz), 7.51–7.31 (m, 5 H), 7.19 (d, 1 H, J=8.5 Hz), 7.17 (d, 2 H, J=8.6 Hz), 7.02 (d, 2 H, J=8.7 Hz), 6.86 (dd; 1 H, J=8.5 Hz, 2.4 Hz), 6.70 (d, 2 H, J=1.8 Hz), 6.63 (dd, 1 H, J=8.7 Hz, 2.4 Hz), 5.86 (s, 1 H), 5.14 (s, 2 H); MS 407 (M−H)−.

후처리

  1. temperatureheated
  2. temperatureto reflux until TLC analysis
  3. customreaction
  4. extractionextracted with EtOAc
  5. washThe EtOAc layer was washed with saturated NaHCO3 aq, brine
  6. dry with materialdried over MgSO4
  7. filtrationAfter filtration
  8. customthe residue was chromatographed on silica gel (1:4 EtOAc/hexanes)

출처 및 근거

ORD 기록
ord-4f0589e03c9b42f0a48dbe9ecefedd7a
출처 데이터셋
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07022733B2

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