Hydrochloric Acid → HCID 20304505、化合物

HRID 236961ノート

反応式

HRID 236961 の反応式
[CH3:1][C:2]1[C:3](=[O:24])[C:4]2[CH:20]=[C:19]3[C:14]([CH2:15][CH2:16][CH2:17][CH2:18]3)=[C:13]([CH2:21][CH2:22][CH3:23])[C:5]=2[O:6][C:7]=1[C:8]([O:10]CC)=[O:9].Cl>C(O)(=O)C>[CH3:1][C:2]1[C:3](=[O:24])[C:4]2[CH:20]=[C:19]3[C:14]([CH2:15][CH2:16][CH2:17][CH2:18]3)=[C:13]([CH2:21][CH2:22][CH3:23])[C:5]=2[O:6][C:7]=1[C:8]([OH:10])=[O:9]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 20304565HCID 20304565、化合物

生成物 1

HCID 20304505HCID 20304505、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of the product of step (f) (16.2 g), glacial acetic acid (80 ml) and 5 N hydrochloric acid (20 ml) was heated and stirred on a steam bath overnight, and then evaporated. The residue was extracted with aqueous sodium bicarbonate and the extract was filtered and then acidified. Precipitated material was isolated by decantation and was triturated with water, dried, then triturated with an ether/petroleum ether (40°-60°) mixture. There remained as an insoluble off-white solid, 6,7,8,9-tetrahydro-3-methyl-4-oxo-10-propyl-4H-naphtho[2,3-b]pyran-2-carboxylic acid, (3.5 g), m.p 162°-4°.

後処理

  1. temperaturewas heated
  2. customevaporated
  3. extractionThe residue was extracted with aqueous sodium bicarbonate
  4. filtrationthe extract was filtered
  5. customPrecipitated material was isolated by decantation
  6. customwas triturated with water
  7. customdried
  8. customtriturated with an ether/petroleum ether (40°-60°) mixture
  9. customremained as an insoluble off-white solid, 6,7,8,9-tetrahydro-3-methyl-4-oxo-10-propyl-4H-naphtho[2,3-b]pyran-2-carboxylic acid, (3.5 g), m.p 162°-4°

出典と根拠

ORDレコード
ord-32a39b1926d9437db97756beeb7c2a2c
出典データセット
uspto-grants-1979_06
特許番号
US04159273

反応ノート

読み込み中…