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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Dicyclohexylcarbodiimide → 9-[4-(Diethylamino)butyryloxy]-1,2-dihydro-4,4-dimethyl-7-(3-methyl-2-octyl)-4H-thieno[2,3-c][1]benzopyran hydrochloride

HRID 1579099
ノート
印刷プレビュー

反応式

HRID 1579099 の反応式
[CH3:1][C:2]1([CH3:25])[C:7]2[S:8][CH2:9][CH2:10][C:6]=2[C:5]2[C:11]([OH:24])=[CH:12][C:13]([CH:15]([CH:17]([CH3:23])[CH2:18][CH2:19][CH2:20][CH2:21][CH3:22])[CH3:16])=[CH:14][C:4]=2[O:3]1.C1(N=C=NC2CCCCC2)CCCCC1.[ClH:41].[CH2:42]([N:44]([CH2:51][CH3:52])[CH2:45][CH2:46][CH2:47][C:48](O)=[O:49])[CH3:43]>C(Cl)Cl>[ClH:41].[CH2:42]([N:44]([CH2:51][CH3:52])[CH2:45][CH2:46][CH2:47][C:48]([O:24][C:11]1[C:5]2[C:6]3[CH2:10][CH2:9][S:8][C:7]=3[C:2]([CH3:1])([CH3:25])[O:3][C:4]=2[CH:14]=[C:13]([CH:15]([CH:17]([CH3:23])[CH2:18][CH2:19][CH2:20][CH2:21][CH3:22])[CH3:16])[CH:12]=1)=[O:49])[CH3:43]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 10868DicyclohexylcarbodiimideHCID 2135232H-Thieno(2,3-c)(1)benzopyran-9-ol, 1,4-dihydro-7-(1,2-dimethylheptyl)-4,4-dimethyl-HCID 137955394-(Diethylamino)butanoic acid hydrochloride

生成物 1

HCID 215579049-[4-(Diethylamino)butyryloxy]-1,2-dihydro-4,4-dimethyl-7-(3-methyl-2-octyl)-4H-thieno[2,3-c][1]benzopyran hydrochloride収率 53%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

0.5 g. (1.39 mmole) of 1,2-dihydro-4,4-dimethyl-9-hydroxy-7-(3-methyl-2-octyl)-4H-thieno[2,3-c][1]benzopyran, 0.31 g. (1.50 mmole; Aldrich Chemical Co.) of dicyclohexylcarbodiimide and 0.272 g. (1.39 mmole) of 4-diethylaminobutyric acid hydrochloride (F. F. Blicke, W. B. Wright, Jr., and M. R. Zienty, J. Amer. Chem. Soc., 63 2488 (1941)) were combined in 30 ml. of methylene chloride and stirred at room temperature for 4 hours. The insoluble by-product of dicyclohexylurea was separated by filtration and the methylene chloride was removed on a rotary evaporator. Attempts to crystallize the material were unsuccessful and 400 mg. (53%) of dark brown residue was obtained. The structure was confirmed by the IR and NMR spectra; and TLC gave Rf 0.5 in 5% MeOH/CHCl3. The acid addition salt may be converted to the free base form by methods well known in the art, and the resulting free base form may then be reacted with another suitable acid to form a different acid addition salt.

後処理

  1. customThe insoluble by-product of dicyclohexylurea was separated by filtration
  2. customthe methylene chloride was removed on a rotary evaporator
  3. customto crystallize the material

出典と根拠

ORDレコード
ord-74df4688fe6b477e9a2eacdf1ef14681
出典データセット
uspto-grants-1976_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03940421

反応ノート

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