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Methanol → HCID 14628047、化合物

HRID 2165936
ノート
印刷プレビュー

反応式

HRID 2165936 の反応式
[C:1]([C:4]1[CH:26]=[CH:25][C:7]([O:8][CH2:9][CH2:10][CH2:11][S:12][C:13]2[NH:14][C:15]3[CH:21]=[C:20]([C:22]([OH:24])=[O:23])[CH:19]=[CH:18][C:16]=3[N:17]=2)=[C:6]([CH2:27][CH2:28][CH3:29])[C:5]=1[OH:30])(=[O:3])[CH3:2].C(N(CC)CC)C.[C:38](OC(=O)C)(=[O:40])[CH3:39].CO>CN(C)C1C=CN=CC=1.ClCCl>[C:38]([O:30][C:5]1[C:6]([CH2:27][CH2:28][CH3:29])=[C:7]([CH:25]=[CH:26][C:4]=1[C:1](=[O:3])[CH3:2])[O:8][CH2:9][CH2:10][CH2:11][S:12][C:13]1[NH:14][C:15]2[CH:21]=[C:20]([C:22]([OH:24])=[O:23])[CH:19]=[CH:18][C:16]=2[N:17]=1)(=[O:40])[CH3:39]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 887MethanolHCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 14628044HCID 14628044、化合物

生成物 1

HCID 14628047HCID 14628047、化合物収率 58.2%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒
HCID 6344
Dichloromethane
溶媒

反応条件

温度
0 °C

実験手順

A mixture of 2-[3-(4-acetyl-3-hydroxy-2-propylphenoxy)-propylthio]benzimidazole-5-carboxylic acid (1.50 g), triethylamine (4 ml), acetic anhydride (4 ml) and 4-dimethylaminopyridine (100 mg) in dichloromethane (50 ml) was stirred at 0 ° C. and then at room temperature for 5 hours. Methanol (4 ml) was added to the mixture, further stirred for an additional 30 minutes and then the mixture was evaporated. The residue was washed with water, dissolved in ethanol, and concentrated to dryness. The residue was purified by silica gel column chromatography, eluting with dichloromethane-ethyl acetate-methanol (10:2:1), and recrystallized from n-hexane-chloroform to give the title compound (970 mg, 58.2%) as yellow crystals, mp 85-87 ° C.

後処理

  1. stirringfurther stirred for an additional 30 minutes
  2. customthe mixture was evaporated
  3. washThe residue was washed with water
  4. dissolutiondissolved in ethanol
  5. concentrationconcentrated to dryness
  6. customThe residue was purified by silica gel column chromatography
  7. washeluting with dichloromethane-ethyl acetate-methanol (10:2:1)
  8. customrecrystallized from n-hexane-chloroform

出典と根拠

ORDレコード
ord-a2ba410fe5704132a3db71ef8a4e6b17
出典データセット
uspto-grants-1990_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04942245

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート