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Ammonium formate → HCID 18926564、化合物

HRID 1600185
ノート
印刷プレビュー

反応式

HRID 1600185 の反応式
[CH3:1][O:2][C:3]([CH2:5][CH2:6][N:7]1[C:15]2[C:10](=[CH:11][C:12](/[CH:16]=[CH:17]/[C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])=[CH:13][CH:14]=2)[C:9]([CH2:25][C:26]2[CH:27]=[N:28][CH:29]=[CH:30][CH:31]=2)=[CH:8]1)=[O:4].C([O-])=O.[NH4+]>[Pd].CO.O1CCCC1>[CH3:1][O:2][C:3]([CH2:5][CH2:6][N:7]1[C:15]2[C:10](=[CH:11][C:12]([CH2:16][CH2:17][C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])=[CH:13][CH:14]=2)[C:9]([CH2:25][C:26]2[CH:27]=[N:28][CH:29]=[CH:30][CH:31]=2)=[CH:8]1)=[O:4]
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

6

反応物 2

HCID 2723923Ammonium formateHCID 86752488HCID 86752488、化合物

生成物 1

HCID 18926564HCID 18926564、化合物収率 98.8%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

A mixture of t-butyl (E)-3-[1-(2-methoxycarbonylethyl)-3-(3-pyridylmethyl)-1H-indol-5-yl]-2-propenoate (7.86 g), 10% palladium on carbon (0.70 g) and ammonium formate (5.60 g) in a mixture of methanol (40 ml) and tetrahydrofuran (40 ml) was heated at 60° C. for 3 hours and then cooled. The mixture was filtered and the residue was washed with methanol. The filtrate and washings were combined and evaporated, and the residue-was partitioned between water and ether. The organic layer was separated and the aqueous layer was extracted with ether. The organic layers were combined, washed with water and dried (MgSO4). Evaporation of the solvent gave the title compound as an oil (7.80 g). Found: C,70.51; H,6.98; N,6.54. C25H30N2O4 requires: C,71.06; H,7.16; N,6.63%.

後処理

  1. temperaturecooled
  2. filtrationThe mixture was filtered
  3. washthe residue was washed with methanol
  4. customevaporated
  5. customthe residue-was partitioned between water and ether
  6. customThe organic layer was separated
  7. extractionthe aqueous layer was extracted with ether
  8. washwashed with water
  9. dry with materialdried (MgSO4)
  10. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-af49b6779c4f4d9393e39a3016248129
出典データセット
uspto-grants-1998_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05744488

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート