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Piperidine, 3,4-didehydro-2,2,6,6-tetramethyl- → HCID 70364728、化合物

HRID 728552
ノート
印刷プレビュー

反応式

HRID 728552 の反応式
CC1(C)CC=CC(C)(C)N1.[C:11]1(=[O:27])[CH2:23][CH2:22][CH:21]2[CH2:24][CH2:25][CH2:26][N:19]3[C:20]2=[C:12]1[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][C:18]=13.C1(C(C2C=CC=CC=2)(C2C=CC=CC=2)[N:35]2[C:39]([CH3:40])=[C:38]([CH:41]=O)[N:37]=[CH:36]2)C=CC=CC=1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>CCCCCC.O1CCCC1.C(O)(=O)C>[CH3:41][C:38]1[NH:37][CH:36]=[N:35][C:39]=1[CH:40]=[C:23]1[CH2:22][CH:21]2[CH2:24][CH2:25][CH2:26][N:19]3[C:20]2=[C:12]([C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][C:18]=23)[C:11]1=[O:27]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 70502Piperidine, 3,4-didehydro-2,2,6,6-tetramethyl-HCID 521998p-Toluenesulfonic acid monohydrateHCID 118243385-methyl-1-trityl-1H-imidazole-4-carbaldehydeHCID 54288891HCID 54288891、化合物

生成物 1

HCID 70364728HCID 70364728、化合物収率 60.7%

試薬・触媒・溶媒 3

HCID 176
Acetic Acid
溶媒
HCID 8028Tetrahydrofuran溶媒3 回
HCID 8058Hexane溶媒

反応条件

温度
0 °C

実験手順

6.88 mmol butyllium in hexane (4.3 ml; 1.6M) were added dropwise at -78° C. to a solution of 1.2 ml (6.88 mmol) of 2,2,6,6-tetramethylpyridine in 14 ml of dry tetrahydrofuran. The mixture was then stirred for 30 minutes at 0° C., cooled to -70° C., and added dropwise to a solution of 1-4 g (6.23 mmol) of 2,3,3a,4,5,6-hexahydro-1H-pyrido[3,2,1-jk]carbazol-1-one in 42 ml of dry tetrahydrofuran. The mixture was stirred for 90 minutes under nitrogen at -70° C. A solution of 2.4 g (6.88 mmol) of 1-triphenylmethyl-5-methyl-1H-imidazole-4-carboxaldehyde in 14 ml of dry tetrahydrofuran was then added dropwise to the reaction mixture at -70° C., and the mixture was stirred for 2 hours at -10° C. The mixture was then cooled to -70° C. and 16.8 ml of acetic acid was added dropwise. After the temperature had raised to -10° C., 8.1 g of p-toluenesulfonic acid hydrate were added. This mixture was boiled for 18 hours and evaporated in vacuum. The residue was shaken with methylene chloride and with 2N sodium hydroxide. The organic layer was separated, washed with brine, dried and evaporated. The residue was chromatographed over silicagel using methylene chloride/methanol/ammonia (92.5/7/0.5) as an eluent. 1.2 g (60%) of 2,3,3a,4,5,6-hexahydro-2-[(5-methyl-1H-imidazol-4-yl)-methylene]-1H- pyrido[3,2,1jk]carbazol-1-one were obtained. This product dissolved in 100 ml of ethanol and hydrogenated at room temperature at 1 atmosphere with palladium on carbon as a catalyst. The catalyst was removed by filtration after disappearance of the starting material, the filtrate was evaporated in vacuum, and the residue was purified by flash chromatography over silicagel using methyene chloride/methanol/ammonia (92.5/7/0.5) as an eluent. 0.49 g of the desired compound were obtained after evaporating the desired fractions.

後処理

  1. temperaturecooled to -70° C.
  2. stirringThe mixture was stirred for 90 minutes under nitrogen at -70° C
  3. stirringthe mixture was stirred for 2 hours at -10° C
  4. temperatureThe mixture was then cooled to -70° C.
  5. temperatureAfter the temperature had raised to -10° C.
  6. waitThis mixture was boiled for 18 hours
  7. customevaporated in vacuum
  8. stirringThe residue was shaken with methylene chloride and with 2N sodium hydroxide
  9. customThe organic layer was separated
  10. washwashed with brine
  11. customdried
  12. customevaporated
  13. customThe residue was chromatographed

出典と根拠

ORDレコード
ord-f04e41a185ee49bfba18f4640cc118ba
出典データセット
uspto-grants-1991_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05049563

反応ノート

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