Bromoform → HCID 21452187, 화합물

HRID 436388

반응식

HRID 436388 반응식
[C:1]1(=O)[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]C1.[OH-].[Na+].C1CCCCCCCCCCC=1.[CH:29]([Br:32])(Br)[Br:30]>[Br-].C[N+](C)(C)C.O>[Br:30][C:29]1([Br:32])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH:12]2[CH:13]1[CH2:1]2

참가 물질

7

반응물 4

HCID 5558BromoformHCID 14798Sodium HydroxideHCID 15164Cyclododecene, (E)-HCID 79114Cyclotridecanone

생성물 1

HCID 21452187HCID 21452187, 화합물수율 92%

시약·촉매·용매 2

HCID 66137Tetramethylammonium bromide촉매HCID 962Water용매

실험 절차

cyclotridecanone: 200 ml of a 50 % aqueous solution of NaOH were added dropwise under vigorous stirring to a mixture of 132 g of cyclododecene (CHEMICAL SAMPLE Co - Columbus, Ohio - USA), 600 g of bromoform and 4 g of tetramethylammonium bromide. The mixture was then left at a temperature between 40° and 50° under stirring during 2 h, whereupon it was left at room temperature overnight and diluted with water. Finally the reaction mixture was extracted with 3 fractions of 300 ml each of ether. The combined extracts, after the usual treatments of washing, drying and evaporation, gave a residue which upon fractional distillation under reduced pressure yielded 173 g (92 %) of 2,2-dibromo-bicyclo[10.1.0]tridecane.

후처리

  1. waitThe mixture was then left at a temperature between 40° and 50°
  2. waitwas left at room temperature overnight
  3. extractionFinally the reaction mixture was extracted with 3 fractions of 300 ml each of ether
  4. washThe combined extracts, after the usual treatments of washing
  5. customdrying
  6. customevaporation
  7. customgave a residue which
  8. distillationupon fractional distillation under reduced pressure

출처 및 근거

ORD 기록
ord-50b3cba028d0444e8df9b173bc48c74d
출처 데이터셋
uspto-grants-1977_02
특허 번호
US04009127

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