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Peracetic Acid → HCID 71281752, 화합물

HRID 1481784
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HRID 1481784 반응식
[CH2:1]([O:8][C:9]1[N:24]=[CH:23][C:22](I)=[C:21]([O:26][CH2:27][C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[C:10]=1[C:11]([O:13][CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=[O:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([Mg]Cl)(C)C.[Li+].[Cl-].B(OC(C)C)(OC(C)C)[O:42]C(C)C.C(OO)(=O)C>C1COCC1.O>[CH2:1]([O:8][C:9]1[N:24]=[CH:23][C:22]([OH:42])=[C:21]([O:26][CH2:27][C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[C:10]=1[C:11]([O:13][CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=[O:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6585Peracetic AcidHCID 21531Triisopropyl borateHCID 71281816HCID 71281816, 화합물HCID 178461733HCID 178461733, 화합물

생성물 1

HCID 71281752HCID 71281752, 화합물수율 36.5%

시약·촉매·용매 2

HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매

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온도
-45 °C

실험 절차

Into a solution of benzyl 2,4-bis(benzyloxy)-5-iodonicotinate (1.0 g, 1.8 mmol) in THF (8.0 mL) at −45° C. was added a solution of i-PrMgCl—LiCl (1.3 M×2.8 mL, 3.6 mmol) dropwise. The mixture was stirred at −45° C. for 30 min, into which triisopropyl borate (0.87 mL, 3.78 mmol) was added dropwise. After stirring at −45° C. for 15 min, the temperature was allowed to rise to room temperature slowly. The mixture was stirred at room temperature for 1.5 h then cooled to −20° C., into which peracetic acid (32%, 0.79 mL, 3.78 mmol) was added. The mixture was stirred at room temperature for another 30 min before it was treated with water (50 mL). The mixture was extracted with ethyl acetate. The organic layers were combined and washed with brine, dried over sodium sulfate, evaporated and purified by silica chromatography (0-30% ethyl acetate in hexanes) to give benzyl 2,4-bis(benzyloxy)-5-hydroxynicotinate (0.29 g, 36%).

후처리

  1. additionwas added dropwise
  2. customto rise to room temperature
  3. stirringThe mixture was stirred at room temperature for 1.5 h
  4. additionwas added
  5. stirringThe mixture was stirred at room temperature for another 30 min before it
  6. extractionThe mixture was extracted with ethyl acetate
  7. washwashed with brine
  8. dry with materialdried over sodium sulfate
  9. customevaporated
  10. custompurified by silica chromatography (0-30% ethyl acetate in hexanes)

출처 및 근거

ORD 기록
ord-32f3dc230177495eada0c348f9c4138f
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09409905B2

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