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

HRID 572696ノート

反応式

HRID 572696 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
215 °C

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-22f87d6074434fb8a5dfa7cbb684a6ce
出典データセット
uspto-grants-2015_05
特許番号
US09029420B2

反応ノート

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