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Ethanol → HCID 89482605, 화합물

HRID 1772188
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HRID 1772188 반응식
[CH3:1][N:2]1[C:6]([NH2:7])=[CH:5][C:4]([CH:8]2[CH2:13][CH2:12][CH2:11][CH2:10][NH:9]2)=[N:3]1.[CH:14]([O:16][CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=[O:15].C(O)C.C1(=O)CCCCC1>C(OCC)(=O)C>[CH3:1][N:2]1[C:6]([NH2:7])=[C:5]([C:18]2[CH2:23][CH2:22][CH2:21][CH2:20][CH:19]=2)[C:4]([CH:8]2[CH2:13][CH2:12][CH2:11][CH2:10][NH:9]2)=[N:3]1.[CH:14]([O:16][CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 702EthanolHCID 7967CyclohexanoneHCID 89482802HCID 89482802, 화합물

생성물 1

HCID 89482605HCID 89482605, 화합물수율 109.1%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

Under nitrogen atmosphere, to a 250 mL three-neck reaction flask were added the compound of Example 11B (11.7 g, 37 mmol), ethanol (150 mL) and cyclohexanone (15.5 mL, 149 mmol). The mixture reacted overnight at 50° C. to 60° C. After cooled to room temperature, acetic acid was removed by rotary-evaporation to obtain a crude product. The crude product was subject to column chromatography (eluant: petroleum ether:ethyl acetate=2:1) to give 8.0 g of the title compound. Yield: 54.4%. MS (ESI): m/z 395 (M+H)+

후처리

  1. customThe mixture reacted overnight at 50° C. to 60° C
  2. customacetic acid was removed by rotary-evaporation
  3. customto obtain a crude product

출처 및 근거

ORD 기록
ord-39b0cbe4a72e4abba51240be667a50d5
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09249172B2

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