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Hydrochloric Acid → HCID 86602944、化合物

HRID 901805
ノート
印刷プレビュー

反応式

HRID 901805 の反応式
[C@@H:1]1([O:12][C@@H:13]2[C@@H:22]([CH2:23][OH:24])[O:21][CH:16]([O:17][CH2:18][CH:19]=[CH2:20])[C@H:15]([OH:25])[C@H:14]2[OH:26])[O:9][C@H:8]([CH2:10][OH:11])[C@@H:6]([OH:7])[C@H:4]([OH:5])[C@H:2]1[OH:3].[C:27](Cl)(=[O:34])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.Cl.CCl>N1C=CC=CC=1>[C:27]([C@@:15]1([OH:25])[C@@:14]([C:27](=[O:34])[C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)([OH:26])[C@H:13]([O:12][C@@H:1]2[O:9][C@H:8]([CH2:10][O:11][C:27](=[O:34])[C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)[C@@H:6]([O:7][C:27](=[O:34])[C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)[C@H:4]([O:5][C:27](=[O:34])[C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)[C@H:2]2[O:3][C:27](=[O:34])[C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[C@@H:22]([CH2:23][O:24][C:27](=[O:34])[C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[O:21][CH:16]1[O:17][CH2:18][CH:19]=[CH2:20])(=[O:34])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6327Methyl ChlorideHCID 7412Benzoyl chlorideHCID 67157178HCID 67157178、化合物

生成物 1

HCID 86602944HCID 86602944、化合物収率 70%

試薬・触媒・溶媒 1

HCID 1049Pyridine
溶媒

実験手順

The compound (4.0 g, 10.46 mmol) synthesized in Example 2 (2a) was dissolved in pyridine (30 mL) and benzoyl chloride (12.1 mL, 104.24 mmol) was added thereto under ice-cooling, followed by stirring of the mixture at room temperature for 14 hours. The reaction mixture was poured to 10% aqueous hydrochloric acid solution (20 mL) and methyl chloride (20 mL) and the organic layer was washed with 10% aqueous hydrochloric acid solution (20 mL), saturated aqueous sodium hydrogencarbonate solution (20 mL) and saturated brine (20 mL) and dried with anhydrous sodium sulfate, followed by distilling off of the solvent under reduced pressure. The residue was purified using silica gel flash column chromatography (hexane:ethyl acetate, 5:1-5:2, V/V) to obtain the desired title compound (8.10 g, yield 70%) as a colorless oil.

後処理

  1. temperatureunder ice-cooling
  2. washthe organic layer was washed with 10% aqueous hydrochloric acid solution (20 mL), saturated aqueous sodium hydrogencarbonate solution (20 mL) and saturated brine (20 mL)
  3. dry with materialdried with anhydrous sodium sulfate
  4. distillationby distilling off of the solvent under reduced pressure
  5. customThe residue was purified

出典と根拠

ORDレコード
ord-aa809817d1264238b2fbebe219cdfd5e
出典データセット
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07361744B2

反応ノート

読み込み中…

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