Hydrochloric Acid → 4-[(5,6,7,8-Tetrahydro-5-hydroxy-8,8-dimethylnaphth-2-yl)ethynyl]benzoic acid

HRID 610315

反応式

HRID 610315 の反応式
[OH:1][CH:2]1[CH2:11][CH2:10][C:9]([CH3:13])([CH3:12])[C:8]2[CH:7]=[C:6]([C:14]#[C:15][C:16]3[CH:26]=[CH:25][C:19]([C:20]([O:22]CC)=[O:21])=[CH:18][CH:17]=3)[CH:5]=[CH:4][C:3]1=2.[Li+].[OH-].Cl>C1COCC1.CO.CCOCC.CCOC(C)=O>[OH:1][CH:2]1[CH2:11][CH2:10][C:9]([CH3:13])([CH3:12])[C:8]2[CH:7]=[C:6]([C:14]#[C:15][C:16]3[CH:17]=[CH:18][C:19]([C:20]([OH:22])=[O:21])=[CH:25][CH:26]=3)[CH:5]=[CH:4][C:3]1=2

参加物

7

反応物 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 15391671Ethyl 4-[(5,6,7,8-tetrahydro-5-hydroxy-8,8-dimethylnaphth-2-yl)ethynyl]benzoate2 回

生成物 1

HCID 183145914-[(5,6,7,8-Tetrahydro-5-hydroxy-8,8-dimethylnaphth-2-yl)ethynyl]benzoic acid

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒HCID 21584169Diethylether ethylacetate溶媒

実験手順

110 mg (0.31 mmol) of ethyl 4-[(5,6,7,8-tetrahydro-5-hydroxy-8,8-dimethylnaphth-2-yl)ethynyl]benzoate (Compound 9) in a mixture of THF and methanol was refluxed with 1 ml (1 mmol) of LiOH (1M aqueous solution). Thereafter the mixture was diluted with Et2O:EtOAc (1:1), and acidified with aqueous HCl to pH 5. The organic phase was separated, washed (water and brine), dried (MgSO4) to yield the title compound.

後処理

  1. customThe organic phase was separated
  2. washwashed (water and brine)
  3. dry with materialdried (MgSO4)

出典と根拠

ORDレコード
ord-238680ad6c1f4fd8aa601d5ddbff7685
出典データセット
uspto-grants-1999_12
特許番号
US05998471

関連ノート

読み込み中…