Sulfur → Ethyl (7-methoxynaphthalen-1-yl)acetate

HRID 572696노트

반응식

HRID 572696 반응식
[S].[CH3:2][O:3][C:4]1[CH:13]=[C:12]2[C:7]([CH2:8][CH2:9][CH2:10][CH:11]2[CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:6][CH:5]=1>C(OCC)(=O)C>[CH2:18]([O:17][C:15](=[O:16])[CH2:14][C:11]1[C:12]2[C:7](=[CH:6][CH:5]=[C:4]([O:3][CH3:2])[CH:13]=2)[CH:8]=[CH:9][CH:10]=1)[CH3:19]

참가 물질

4

반응물 2

HCID 5362487SulfurHCID 15720546Ethyl (1,2,3,4-tetrahydro-7-methoxy-1-naphthyl)acetate

생성물 1

HCID 13570063Ethyl (7-methoxynaphthalen-1-yl)acetate수율 103.9%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
215 °C

실험 절차

17.6 g sulfur and 90 g ethyl (7-methoxy-1,2,3,4-tetrahydro-1-naphthalenyl)-acetate were added into the reaction flask and heated to 215° C. with stirring. The reaction was carried out for 10 hours. After completion of the reaction, the reaction system was cooled to 60° C. 500 ml ethyl acetate was added and the mixture was stirred for 30 minutes. The mixture was filtered and the filter cake was washed with 100 ml ethyl acetate. Then, the filtrate was combined and vacuum evaporated to obtain 92 g brown oil with 82.4% content (HPLC). The yield is 85%.

후처리

  1. customAfter completion of the reaction
  2. temperaturethe reaction system was cooled to 60° C
  3. stirringthe mixture was stirred for 30 minutes
  4. filtrationThe mixture was filtered
  5. washthe filter cake was washed with 100 ml ethyl acetate
  6. customvacuum evaporated

출처 및 근거

ORD 기록
ord-22f87d6074434fb8a5dfa7cbb684a6ce
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09029420B2

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