Toluene → HCID 22285400, 화합물

HRID 1689751

반응식

HRID 1689751 반응식
[C:1]1([CH3:7])[CH:6]=[CH:5]C=CC=1.[H-].[Na+].[S:10]1[CH2:15][CH2:14][CH2:13][S:12][CH:11]1[C:16]([O:18][CH2:19][CH3:20])=[O:17].BrCC1CC1>CN(C=O)C>[CH2:19]([O:18][C:16]([C:11]1([CH2:7][CH:1]2[CH2:6][CH2:5]2)[S:12][CH2:13][CH2:14][CH2:15][S:10]1)=[O:17])[CH3:20]

참가 물질

6

반응물 4

HCID 1140TolueneHCID 24758Sodium hydrideHCID 81503BromomethylcyclopropaneHCID 88552Ethyl 1,3-dithiane-2-carboxylate

생성물 1

HCID 22285400HCID 22285400, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a flamed dried flask is added dry toluene (80 mL) and sodium hydride (60%, 33.5 mmol, 1.34 g). The reaction is cooled in a ice bath and a solution of ethyl 1,3 dithiane carboxylate (52 mmol, 10 g) and bromomethyl cyclopropane (62.4 mmol, 8.42 g) in DMF (24 mL) are added dropwise over 10 minutes. The ice bath is removed and the reaction is stirred for 18 h. Water is added (50 mL) and the organic layer is separated. The organic layer is washed with brine, dried (Na2SO4), and concentrated to a yellow oil (12 g, 92%). LC-ES/MS: 247.0 (M+1).

후처리

  1. customTo a flamed dried flask
  2. temperatureThe reaction is cooled in a ice bath
  3. customThe ice bath is removed
  4. additionWater is added (50 mL)
  5. customthe organic layer is separated
  6. washThe organic layer is washed with brine
  7. dry with materialdried (Na2SO4)
  8. concentrationconcentrated to a yellow oil (12 g, 92%)

출처 및 근거

ORD 기록
ord-2b7089650b25413781be88d029022323
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08153624B2

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