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Hydrochloric Acid → HCID 178489059, 화합물

HRID 2174140
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HRID 2174140 반응식
[C:1]([C:3]1[CH:39]=[CH:38][C:6]2[N:7](COCC[Si](C)(C)C)[C:8]([CH2:10][C:11]3[C:19]([O:20][CH3:21])=[CH:18][C:17]([CH3:22])=[C:16]4[C:12]=3[CH:13]=[CH:14][N:15]4C(OC(C)(C)C)=O)=[N:9][C:5]=2[CH:4]=1)#[N:2].C(C1C=CC2N=C(CC3C(OC)=CC(C)=C4C=3C=CN4C(OC(C)(C)C)=O)N(COCC[Si](C)(C)C)C=2C=1)#N.[Li+].CC([N-]C(C)C)C.I[CH2:88][CH2:89][CH2:90][C:91]([O:93]C)=[O:92].C(=O)([O-])[O-].[K+].[K+].Cl>C1COCC1.CO.O>[C:1]([C:3]1[CH:39]=[CH:38][C:6]2[NH:7][C:8]([CH:10]([C:11]3[C:19]([O:20][CH3:21])=[CH:18][C:17]([CH3:22])=[C:16]4[C:12]=3[CH:13]=[CH:14][NH:15]4)[CH2:88][CH2:89][CH2:90][C:91]([OH:93])=[O:92])=[N:9][C:5]=2[CH:4]=1)#[N:2]
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참가 물질

10

반응물 6

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 547991Methyl 4-iodobutanoateHCID 2724682Lithium diisopropylamideHCID 86701791HCID 86701791, 화합물HCID 86701792HCID 86701792, 화합물

생성물 1

HCID 178489059
HCID 178489059, 화합물

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매

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온도
65 °C

실험 절차

tert-Butyl 4-((5-cyano-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-benzo[d]imidazol-2-yl)methyl)-5-methoxy-7-methyl-1H-indole-1-carboxylate and tert-butyl 4-((6-cyano-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-benzo[d]imidazol-2-yl)methyl)-5-methoxy-7-methyl-1H-indole-1-carboxylate (Example 145-A) (510 mg, 0.93 mmol) in THF (10 mL) was stirred at −78° C. and then LDA (2.0M in heptane/THF/ethylbenzene, 0.47 mL, 0.93 mmol) was added and the reaction was stirred for 10 minutes. At this point, methyl 4-iodobutanoate (0.5 mL, 3.7 mmol) was added and the dry ice bath was removed and the reaction was stirred for 2.5 hours at rt. The reaction was diluted with ethyl acetate (100 mL) and poured into saturated aq. solution of sodium chloride. The layers were separated and the organic layer was dried over Na2SO4, concentrated and absorbed onto silica to purify via FCC (0-20% EtOAc:hexanes). The resulting residue was deprotected of the SEM and Boc group using the conditions shown in Example 142-C. The resulting residue (170 mg, 0.408 mmol) was dissolved in MeOH (5 mL) and was added potassium carbonate (180 mg, 1.3 mmol), the reaction was heated at 65° C. overnight. The mixture was then poured into water (50 mL) and the pH was adjusted to −1 with 3 M HCl. The layers were separated and the aqueous layer was extracted with ethyl acetate, dried over Na2SO4, and purified by reverse-phase FCC (0-50%) ACN:water to obtain the title compound. 1H NMR (400 MHz, DMSO-d6) δ ppm 12.04-12.24 (m, 1H) 11.86-12.03 (m, 1H) 10.88 (s, 1H) 7.93-8.22 (m, 1H) 7.63-7.83 (m, 1H) 7.36-7.52 (m, 1H) 7.12 (t, J=2.81 Hz, 1H) 6.79 (s, 1H) 6.05 (br. s., 1H) 4.87 (dd, J=9.41, 5.62 Hz, 1H) 3.76 (s, 3H) 2.52-2.59 (m, 1H) 2.45 (s, 3H) 2.03-2.30 (m, 3H) 1.48-1.64 (m, 1H) 1.30-1.46 (m, 1H). HRMS calcd. for C23H22N4O3 (M+H)+ 403.1770. found 403.1758.

후처리

  1. customthe dry ice bath was removed
  2. stirringthe reaction was stirred for 2.5 hours at rt
  3. additionThe reaction was diluted with ethyl acetate (100 mL)
  4. additionpoured into saturated aq. solution of sodium chloride
  5. customThe layers were separated
  6. dry with materialthe organic layer was dried over Na2SO4
  7. concentrationconcentrated
  8. customabsorbed onto silica
  9. customto purify via FCC (0-20% EtOAc:hexanes)
  10. customThe layers were separated
  11. extractionthe aqueous layer was extracted with ethyl acetate
  12. dry with materialdried over Na2SO4
  13. custompurified by reverse-phase FCC (0-50%) ACN

출처 및 근거

ORD 기록
ord-0b82513fae6e43ba8a5851b0d62b03ba
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09056874B2

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