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Triethylamine → HCID 18918517、化合物

HRID 1290479
ノート
印刷プレビュー

反応式

HRID 1290479 の反応式
Cl.Cl.[N:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:14][CH2:13][N:12]([CH2:15][C:16]([OH:18])=O)[CH2:11][CH2:10]2)=[CH:5][CH:4]=1.[CH2:19](N(CC)CC)[CH3:20].C1C=CC2N(O)N=NC=2C=1.C(N=C=NC(C)C)(C)C.C([N:47]1[CH2:52][CH2:51][CH:50]([CH2:53][C:54]([OH:56])=[O:55])[CH2:49][CH2:48]1)C>CN(C)C=O>[N:3]1[CH:4]=[CH:5][C:6]([N:9]2[CH2:10][CH2:11][N:12]([CH2:15][C:16]([N:47]3[CH2:48][CH2:49][CH:50]([CH2:53][C:54]([O:56][CH2:19][CH3:20])=[O:55])[CH2:51][CH2:52]3)=[O:18])[CH2:13][CH2:14]2)=[CH:7][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 8471TriethylamineHCID 12734DiisopropylcarbodiimideHCID 757711-HydroxybenzotriazoleHCID 18918276(1-Ethylpiperidin-4-yl)acetic acidHCID 189185271-Piperazineacetic acid, 4-(4-pyridinyl)-, hydrochloride (1:2)

生成物 1

HCID 18918517HCID 18918517、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution containing 1-(4-pyridyl)-4-carboxymethylpiperazine dihydrochloride 1/4H2O(400 mg, 1.33 mMoles), triethylamine (0.4 ml, 2.66 mMoles) and HOBT (0.2 g, 1.46 mMoles) in dry dimethylformamide (20 ml) was treated with diisopropylcarbodiimide (0.23 ml 1.46 mMoles) and the mixture was stirred for 5 minutes. Ethyl 4-carboxymethylpiperidine was added and the mixture was stirred for a further 4 hours. The mixture was concentrated to half volume under reduced pressure and then poured into water (50 ml) and extracted with ethyl acetate (3×20 ml) and dichloromethane (3×20 ml). The combined organic extracts were concentrated under reduced pressure and the residue was purified by chromatography (flash column made with grade III alumina and eluted with a gradient of 0-1% methanol in dichloromethane) to give the title compound (130 mg) as a colourless oil; NMR (d6DMSO) 0.9-1.1 (m,2H), 1.2(t,3H), 1.65(d,2H), 1.8-2.0(m,1H), 2.2(d,2H), 2.5(m,2H), 2.9-3.4(m,10H), 4.0(q,2H +m,1H), 4.3(d,1H), 6.8(d,2H ), 8.15(d,2H); m/e 375 (M+H)+.

後処理

  1. stirringthe mixture was stirred for a further 4 hours
  2. concentrationThe mixture was concentrated to half volume under reduced pressure
  3. additionpoured into water (50 ml)
  4. extractionextracted with ethyl acetate (3×20 ml) and dichloromethane (3×20 ml)
  5. concentrationThe combined organic extracts were concentrated under reduced pressure
  6. customthe residue was purified by chromatography (flash column
  7. washeluted with a gradient of 0-1% methanol in dichloromethane)

出典と根拠

ORDレコード
ord-be0a7dec23794f8ebc84c1a8a9159d6f
出典データセット
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05750754

反応ノート

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