Sulfuric Acid → HCID 67053816, 화합물

HRID 2171733노트

반응식

HRID 2171733 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 67053816HCID 67053816, 화합물수율 89%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-84a60f795a234838a54cc47bf8638ed0
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09051331B2

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