Dibah → 7-(9H-Fluoren-2-yl)-7,9-diaza-bicyclo[4.2.2]dec-3-ene

HRID 40626

반응식

HRID 40626 반응식
[CH:1]1[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][C:2]=1[N:14]1[C:21](=O)[CH:20]2[NH:23][C:24](=O)[CH:15]1[CH2:16][CH:17]=[CH:18][CH2:19]2.CC(C[Al]CC(C)C)C>C1COCC1.C(OCC)C>[CH:1]1[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][C:2]=1[N:14]1[CH2:21][CH:20]2[NH:23][CH2:24][CH:15]1[CH2:16][CH:17]=[CH:18][CH2:19]2

참가 물질

5

반응물 2

HCID 16682954DibahHCID 692333837-(9H-Fluoren-2-yl)-7,9-diaza-bicyclo[4.2.2]dec-3-ene-8,10-dione

생성물 1

HCID 692339867-(9H-Fluoren-2-yl)-7,9-diaza-bicyclo[4.2.2]dec-3-ene

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
130 °C

실험 절차

7-(9H-Fluoren-2-yl)-7,9-diaza-bicyclo[4.2.2]dec-3-ene-8,10-dione (310 mg, 0.94 mmol) in THF (4 mL) was placed in a μW tube. Dibal-H (4 mL, 4 mmol, [1M] in THF) was then added to the reaction mixture with venting under argon flow. When all H2 evolution was completed, the reaction mixture was heated to 130° C. for 900 sec. The reaction mixture was then diluted with a saturated Rochelle's solution (30 mL) and diethyl ether (30 mL) followed by stirring vigorously overnight. The layers were separated and the organic solution was dried with magnesium sulfate, filtered and the solvent removed by reduced pressure to yield the title compound as a residue.

후처리

  1. customThe layers were separated
  2. dry with materialthe organic solution was dried with magnesium sulfate
  3. filtrationfiltered
  4. customthe solvent removed by reduced pressure

출처 및 근거

ORD 기록
ord-8cee26150f8d4837884a2005f2ecc90d
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08530475B2

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