Hydrochloric Acid → HCID 20336130、化合物

HRID 1706503ノート

反応式

HRID 1706503 の反応式
[H-].[Na+].[CH2:3]([O:5]C=O)[CH3:4].[CH3:8][C:9]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([CH3:13])[C:10](=[O:12])C.Cl>CCOCC.C1C=CC=CC=1>[CH3:13][C:9]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([CH3:8])[C:10](=[O:12])[CH2:4][CH:3]=[O:5]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 8025Ethyl formateHCID 24758Sodium hydrideHCID 2854623-Methyl-3-phenylbutan-2-one

生成物 1

HCID 20336130HCID 20336130、化合物

試薬・触媒・溶媒 2

HCID 241Benzene溶媒3 回HCID 3283Diethyl Ether溶媒

反応条件

温度
40 °C

実験手順

A mixture of 8.8 g. of 50% NaH oil dispersion in 150 ml. of dry benzene was treated at 25° C. with 13.6 g. of ethylformate in 20 ml. of dry benzene under N2. Over a period of a half hour, 14.9 g. of 3-methyl-3-phenyl-2-butanone in 80 ml. of dry benzene was added at 0° C. After stirring at 40° C. for 4 hours, the mixture was diluted with 250 ml. of ether, treated with ice and acidified with hydrochloric acid. The acidic solution ws extracted with ether and the ether extract was washed with brine, sodiuim bicarbonate solution, washed again with brine and dried. The solvent was evaporated and the residue was distilled under reduced pressure to afford 14.8 g. of the title product as an oil, B. P. 83°-84°/0.2 mm., λmaxfilm 3.5 (broad) 5.75, 5.90, 6.12, 6.30, 6.70, 6.80, 6.95, 7.31, 7.94, 8.18, 9,38, 12,60, 13.05 and 14.28 μ.

後処理

  1. additionA mixture of 8.8 g
  2. waitOver a period of a half hour
  3. additionthe mixture was diluted with 250 ml
  4. extractionThe acidic solution ws extracted with ether
  5. extractionthe ether extract
  6. washwas washed with brine, sodiuim bicarbonate solution
  7. washwashed again with brine
  8. customdried
  9. customThe solvent was evaporated
  10. distillationthe residue was distilled under reduced pressure
  11. customto afford 14.8 g

出典と根拠

ORDレコード
ord-75b86eea38344e03b53276e3cec65a0b
出典データセット
uspto-grants-1980_06
特許番号
US04207419

反応ノート

読み込み中…