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

HRID 40626

反応式

HRID 40626 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
130 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8cee26150f8d4837884a2005f2ecc90d
出典データセット
uspto-grants-2013_09
特許番号
US08530475B2

関連ノート

読み込み中…