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HCID 66718591, 화합물 → HCID 66718751, 화합물

HRID 1690806
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HRID 1690806 반응식
C([O:8][CH2:9][CH:10]1[CH2:23][O:22][C:13]2=[N:14][C:15]([C:18]([F:21])([F:20])[F:19])=[CH:16][CH:17]=[C:12]2[O:11]1)C1C=CC=CC=1>C(O)C.[Pd]>[F:21][C:18]([F:19])([F:20])[C:15]1[N:14]=[C:13]2[O:22][CH2:23][CH:10]([CH2:9][OH:8])[O:11][C:12]2=[CH:17][CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 66718591HCID 66718591, 화합물

생성물 1

HCID 66718751HCID 66718751, 화합물수율 81.8%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

To a stirred solution of 2-benzyloxymethyl-6-trifluoromethyl-2,3-dihydro[1,4]dioxino[2,3-b]pyridine (420 mg, 1.3 mmol) in ethanol (50 mL) was added 10% palladium on carbon (10 mg, cat.). The reaction mixture was evacuated and purged with hydrogen six times, then stirred for 3 hours under a hydrogen atmosphere. The reaction mixture was filtered through celite, washing with EtOH (60 mL), and the filtrate evaporated to dryness. Trituration using DCM/hexanes gave the title compound (250 mg, 78%) as a solid. m/z=236.2 (M+1), r.t.=2.46 mins. 1H NMR (400 MHz; CDCl3) δ7.38-7.28 (2H, m), 4.50-4.46 (1H, m), 4.41 (1H, dd), 4.20 (1H, dd), 4.04 (1H, dd), 3.90 (1H, dd).

후처리

  1. customThe reaction mixture was evacuated
  2. custompurged with hydrogen six times
  3. filtrationThe reaction mixture was filtered through celite
  4. washwashing with EtOH (60 mL)
  5. customthe filtrate evaporated to dryness

출처 및 근거

ORD 기록
ord-c6371fd7945b4d1686952bc3e8308366
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08153651B2

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