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HCID 68002031, 화합물 → HCID 86660602, 화합물

HRID 2046025
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HRID 2046025 반응식
[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([C:13]2[O:17][N:16]=[C:15]([C:18]3[CH:19]=[CH:20][C:21]4[O:25][C:24]([CH:26]([OH:28])C)=[CH:23][C:22]=4[CH:29]=3)[N:14]=2)[CH:7]=[CH:8][C:9]=1[O:10][CH2:11][CH3:12])[CH3:2]>O1CCOCC1.O=[Mn]=O>[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([C:13]2[O:17][N:16]=[C:15]([C:18]3[CH:19]=[CH:20][C:21]4[O:25][C:24]([CH:26]=[O:28])=[CH:23][C:22]=4[CH:29]=3)[N:14]=2)[CH:7]=[CH:8][C:9]=1[O:10][CH2:11][CH3:12])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 68002031HCID 68002031, 화합물

생성물 1

HCID 86660602HCID 86660602, 화합물수율 101.1%

시약·촉매·용매 2

HCID 14801Manganese dioxide촉매HCID 312751,4-Dioxane용매

실험 절차

A suspension of the product of Step D (0.13 g; 0.34 mmol) and MnO2 (0.15 g; 1.7 mmol) in dioxane (4 ml) was refluxed for 1 h with stirring. After cooling to room temperature, the insoluble material was removed by filtration, washed with EtOAc (20 ml) and combined filtrates were evaporated to dryness to give the title compound (0.13 g; 100%), as greyish solid. 1H-NMR (CDCl3) 9.91 (s, 1H); 8.59 (s, 1H); 8.33 (dd, 1H, J=2, 9 Hz); 7.63-7.82 (m, 4H); 6.99 (d, 1H, J=9 Hz); 4.14-4.26 (m, 4H); 1.4-1.57 (m, 6H+H2O).

후처리

  1. temperaturewas refluxed for 1 h
  2. customthe insoluble material was removed by filtration
  3. washwashed with EtOAc (20 ml)
  4. customwere evaporated to dryness

출처 및 근거

ORD 기록
ord-514a75a8a3134120a06ce185769a3477
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08592399B2

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