Sulfuric Acid → HCID 67053816、化合物

HRID 2171733ノート

反応式

HRID 2171733 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[C:8]([CH3:13])([CH3:12])[CH2:7][CH2:6]2.C1C(=O)N([Br:21])C(=O)C1.OS(O)(=O)=O>O>[Br:21][C:11]1[CH:10]=[C:9]2[C:5]([CH2:6][CH2:7][C:8]2([CH3:13])[CH3:12])=[CH:4][C:3]=1[O:2][CH3:1]

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 67184N-bromobutanimideHCID 221522852,3-Dihydro-5-methoxy-1,1-dimethyl-1H-indene

生成物 1

HCID 67053816HCID 67053816、化合物収率 89%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

To a suspension of 5-methoxy-1,1-dimethyl-indan (2.16 g, 12.25 mmol) (prepared following the procedures described in U.S. Pat. Appl. Publ., 2006100460) in water (120 ml), NBS (2.2 g, 12.3 mmol) was added. The reaction mixture was heated to 60° C. while stirring. Concentrated H2SO4 (1.3 ml, 40% aq. solution) was then added and stirring was continued for 5 hours. The reaction mixture was cooled to rt. The mixture was extracted with diethyl ether three times. The combined organic extract was washed with brine and dried (Na2SO4). Silica gel chromatography (ethyl acetate/heptane) provided 2.78 g (89%) of the title compound.

後処理

  1. customprepared
  2. stirringstirring
  3. temperatureThe reaction mixture was cooled to rt
  4. extractionThe mixture was extracted with diethyl ether three times
  5. extractionThe combined organic extract
  6. washwas washed with brine
  7. dry with materialdried (Na2SO4)

出典と根拠

ORDレコード
ord-84a60f795a234838a54cc47bf8638ed0
出典データセット
uspto-grants-2015_06
特許番号
US09051331B2

反応ノート

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