Acetic Anhydride → HCID 178478895、化合物

HRID 1253261

反応式

HRID 1253261 の反応式
[CH:1]1([C:9]([OH:11])=[O:10])[CH2:5][CH2:4][CH:3]([C:6]([OH:8])=O)[CH2:2]1.C(OC(=O)C)(=O)C.[ClH:19].[NH2:20][CH2:21][CH2:22][CH2:23][CH2:24][N:25]1[CH2:30][CH2:29][N:28]([CH2:31][C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[CH2:27][CH2:26]1.C(N(CC)CC)C>O.C1(C)C(C)=CC=CC=1>[ClH:19].[ClH:19].[CH2:31]([N:28]1[CH2:27][CH2:26][N:25]([CH2:24][CH2:23][CH2:22][CH2:21][N:20]=[C:6]([CH:3]2[CH2:4][CH2:5][CH:1]([C:9]([OH:11])=[O:10])[CH2:2]2)[OH:8])[CH2:30][CH2:29]1)[C:32]1[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=1

参加物

7

反応物 4

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 1072161,3-Cyclopentanedicarboxylic acidHCID 201374991-(4-Aminobutyl)-4-benzylpiperazine hydrochloride

生成物 1

HCID 178478895HCID 178478895、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 7237O-Xylene溶媒

実験手順

1,3-Cyclopentane dicarboxylic acid (8.0 g., 51 mmole) was converted to the anhydride by refluxing for 3 hours in 100 ml. of acetic anhydride. The excess solvent was removed under vacuum and the residue was stored in vacuum for 18 hours. The crude anhydride thus obtained was combined with 14 g. (50 mmole) of 1-(4-aminobutyl)-4-benzylpiperazine hydrochloride and 5.0 g. (50 mmole) of triethylamine in 500 ml. of xylene. The mixture was refluxed for 48 hours with water separation via a Dean-Stark trap. The product was concentrated under vacuum and chromatographed on 200 g. of silica gel with 2% ethanol/chloroform. The product was crystallized from ethanol by addition of 4N HCl/isopropyl alcohol to obtain cyclopentane-1,3-dicarboxylic-N-[4-(4-benzyl-1-piperazinyl)butyl]imide dihydrochloride; m.p. 273°-275° C.

後処理

  1. temperatureby refluxing for 3 hours in 100 ml
  2. customThe excess solvent was removed under vacuum
  3. customThe crude anhydride thus obtained
  4. concentrationThe product was concentrated under vacuum
  5. customchromatographed on 200 g
  6. customThe product was crystallized from ethanol by addition of 4N HCl/isopropyl alcohol

出典と根拠

ORDレコード
ord-08521a6b0d0b4fd3934f670411b3b9a9
出典データセット
uspto-grants-1988_05
特許番号
US04748240

関連ノート

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