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Potassium Carbonate → HCID 68677180, 화합물

HRID 1158512
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HRID 1158512 반응식
[CH3:1][O:2][C:3](=[O:41])[NH:4][C@H:5]([C:10]([NH:12][NH:13][CH2:14][CH2:15][C@:16]([CH2:34][C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1)([OH:33])[C:17]([N:19]1[C@H:23]2[C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][C:29]=3[CH2:30][C@H:22]2[O:21]C1(C)C)=[O:18])=[O:11])[C:6]([CH3:9])([CH3:8])[CH3:7].C([O-])([O-])=O.[K+].[K+].[Br:48][C:49]1[CH:56]=[CH:55][C:52]([CH2:53]Br)=[CH:51][CH:50]=1>CC(=O)CC>[CH3:1][O:2][C:3](=[O:41])[NH:4][C@@H:5]([C:10]([NH:12][N:13]([CH2:53][C:52]1[CH:55]=[CH:56][C:49]([Br:48])=[CH:50][CH:51]=1)[CH2:14][CH2:15][C@@:16]([OH:33])([C:17](=[O:18])[NH:19][C@H:23]1[C:24]2[C:29](=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH2:30][C@H:22]1[OH:21])[CH2:34][C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1)=[O:11])[C:6]([CH3:7])([CH3:9])[CH3:8]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 685274-Bromobenzyl bromideHCID 68676597HCID 68676597, 화합물

생성물 1

HCID 68677180HCID 68677180, 화합물

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

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온도
80 °C

실험 절차

Compound 21i (0.105 g) was dissolved in 2-butanone (10 mL) and added K2CO3 (0.045 g, 0.32 mmol), and 4-bromobenzyl bromide (0.054 g, 0.21 mmol) and stirred at 80° C. for 3 h. Solvent was evaporated and the residue was dissolved in dichloromethane (15 mL), washed with water, brine and cooled to 0° C. TFA (1.0 mL) was added slowly and stirred for 30 min then evaporated. Residue dissolved in dichloromethane (10 mL) and washed with NaHCO3 solution, water, brine and dried. Residue was purified by analytical preparative LCMS to yield 0.023 g (15% overall yield) of the title compound.

후처리

  1. customSolvent was evaporated
  2. dissolutionthe residue was dissolved in dichloromethane (15 mL)
  3. washwashed with water, brine
  4. temperaturecooled to 0° C
  5. additionTFA (1.0 mL) was added slowly
  6. stirringstirred for 30 min
  7. customthen evaporated
  8. dissolutionResidue dissolved in dichloromethane (10 mL)
  9. washwashed with NaHCO3 solution, water, brine
  10. customdried
  11. customResidue was purified by analytical preparative LCMS
  12. customto yield

출처 및 근거

ORD 기록
ord-a0e74bf6989d48b1af6572493d9a6286
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07807677B2

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