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Acetic Anhydride → HCID 69497897、化合物

HRID 460643
ノート
印刷プレビュー

反応式

HRID 460643 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:9]2[CH2:14][CH2:13][N:12]([CH2:15][C@H:16]([OH:34])[CH2:17][O:18][C:19]3[C:27]4[CH:26]=[C:25]([C:28]5[O:29][C:30]([CH3:33])=[N:31][N:32]=5)[O:24][C:23]=4[CH:22]=[CH:21][CH:20]=3)[CH2:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8].[C:35](OC(=O)C)(=[O:37])[CH3:36]>N1C=CC=CC=1>[ClH:1].[C:35]([O:34][C@@H:16]([CH2:15][N:12]1[CH2:11][CH2:10][CH:9]([C:4]2[CH:5]=[CH:6][C:7]([Cl:8])=[C:2]([Cl:1])[CH:3]=2)[CH2:14][CH2:13]1)[CH2:17][O:18][C:19]1[C:27]2[CH:26]=[C:25]([C:28]3[O:29][C:30]([CH3:33])=[N:31][N:32]=3)[O:24][C:23]=2[CH:22]=[CH:21][CH:20]=1)(=[O:37])[CH3:36]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 9806065MIN-117

生成物 1

HCID 69497897HCID 69497897、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

(S)-1-(4-(3,4-Dichlorophenyl)piperidino)-3-(2-(5-methyl-1,3,4-oxadiazol-2-yl)benzo(b)furan-4-yloxy)-2-propanol (1.0 g) was dissolved in pyridine (20 ml) and acetic anhydride (10 ml), and the mixture was left standing at room temperature for 12 hr. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (chloroform/methanol). The obtained oil was dissolved in ethanol and a solution of hydrogen chloride in ether was added. The precipitated crystals were collected by filtration and dried to give the title compound (0.58 g) as pale-yellow crystals, melting point 163–166° C. (decomposition)

後処理

  1. customThe solvent was evaporated under reduced pressure
  2. customthe residue was purified by silica gel column chromatography (chloroform/methanol)
  3. dissolutionThe obtained oil was dissolved in ethanol
  4. additiona solution of hydrogen chloride in ether was added
  5. filtrationThe precipitated crystals were collected by filtration
  6. customdried

出典と根拠

ORDレコード
ord-bc1aa9e658ef4ceb8ac4c23e21ab2830
出典データセット
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07196199B2

反応ノート

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