Sodium Hydroxide → HCID 59561114、化合物

HRID 1918435ノート

反応式

HRID 1918435 の反応式
[CH3:1][C:2]1[C:14]2[C:13](=O)[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][C:11]=3[CH3:16])[C:6]=2[CH:5]=[C:4]([CH3:17])[CH:3]=1.I.[OH-].[Na+]>C(O)(=O)CC.O>[CH3:1][C:2]1[C:14]2[CH2:13][C:12]3[C:7](=[CH:8][CH:9]=[CH:10][C:11]=3[CH3:16])[C:6]=2[CH:5]=[C:4]([CH3:17])[CH:3]=1

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 24841Hydrogen iodideHCID 57909153HCID 57909153、化合物2 回

生成物 1

HCID 59561114HCID 59561114、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1032Propionic Acid溶媒

実験手順

1,3,8-Trimethylfluoren-9-one (53) was reduced according to the general procedure of Carruthers et al. (W. Carruthers, D. Whitmarsh, J. Chem. Soc. Perkin Trans, I 1973, 1511). 1,3,8-Trimethylfluoren-9-one (53) (2.74 g, 12.3 mmol) was dissolved in propionic acid (235 ml). Red phosphorus (3.0 g) and concentrated HI (40 ml) were added and the reaction mixture was refluxed for 24 h. Quantitative conversion was shown by TLC. The reaction mixture was diluted with water (250 ml), neutralized with NaOH and extracted with Et2O (4×125 ml). The combined organic layers were washed with brine (2×125 ml), dried over MgSO4, filtered and the volatiles removed in vacuo to afford 2.56 g (quant.) 54 as a white solid.

後処理

  1. temperaturethe reaction mixture was refluxed for 24 h
  2. extractionextracted with Et2O (4×125 ml)
  3. washThe combined organic layers were washed with brine (2×125 ml)
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customthe volatiles removed in vacuo

出典と根拠

ORDレコード
ord-3df40ec1fed24af089656ebffef515d4
出典データセット
uspto-grants-2013_12
特許番号
US08618328B2

反応ノート

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