Lithium Hydroxide → 4-[2,2-Dimethyl-4-(5-methyl-thiophen-2-yl)-2H-benzo[g]chromen-7-yl]-benzoic acid

HRID 2288315

反応式

HRID 2288315 の反応式
C([O:3][C:4](=[O:33])[C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:12]=[CH:13][C:14]3[CH:23]=[C:22]4[C:17]([C:18]([C:26]5[S:27][C:28]([CH3:31])=[CH:29][CH:30]=5)=[CH:19][C:20]([CH3:25])([CH3:24])[O:21]4)=[CH:16][C:15]=3[CH:32]=2)=[CH:7][CH:6]=1)C.[Li+].[OH-]>CO.C1COCC1.O>[CH3:24][C:20]1([CH3:25])[CH:19]=[C:18]([C:26]2[S:27][C:28]([CH3:31])=[CH:29][CH:30]=2)[C:17]2[C:22](=[CH:23][C:14]3[CH:13]=[CH:12][C:11]([C:8]4[CH:9]=[CH:10][C:5]([C:4]([OH:33])=[O:3])=[CH:6][CH:7]=4)=[CH:32][C:15]=3[CH:16]=2)[O:21]1

参加物

6

反応物 2

HCID 3939Lithium HydroxideHCID 15887284Ethyl4-[2,2-dimethyl-4-(5-methyl-thien-2-yl)-benzo[1,2-g]-chrom-3-en-7-yl]benzoate2 回

生成物 1

HCID 98453824-[2,2-Dimethyl-4-(5-methyl-thiophen-2-yl)-2H-benzo[g]chromen-7-yl]-benzoic acid

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of ethyl-4-[2,2-dimethyl-4-(5-methyl-thien-2-yl)-benzo[1,2-g]-chrom-3-en-7-yl]benzoate (Compound 11, 18 mg, 0.03 mmol) in methanol (0.5 mL) and THF (1 mL), was added LiOH in water (1M solution, 0.3 mL). The reaction mixture was stirred for 20 hours, the solvent was removed under reduced pressure, the residue dissolved in water (5 mL), washed with ether (10 mL) and the aqueous layer was acidified to PH 5. The aqueous layer was extracted with ethyl acetate (3×20 mL). The combined organic layers were washed with brine, dried, and the solvent was removed under reduced pressure to afford the title compound as a pale yellow solid.

後処理

  1. customthe solvent was removed under reduced pressure
  2. dissolutionthe residue dissolved in water (5 mL)
  3. washwashed with ether (10 mL)
  4. extractionThe aqueous layer was extracted with ethyl acetate (3×20 mL)
  5. washThe combined organic layers were washed with brine
  6. customdried
  7. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-ad41243b5cfb452aaa8cf97d3786b542
出典データセット
uspto-grants-2000_07
特許番号
US06087505

関連ノート

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