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Ethyl Acetate → HCID 69550120、化合物

HRID 2214821
ノート
印刷プレビュー

反応式

HRID 2214821 の反応式
Cl.Cl.[NH2:3][C:4]1([CH2:16][N:17]2[CH2:22][CH2:21][N:20]([S:23]([C:26]3[CH:35]=[CH:34][C:33]4[C:28](=[CH:29][CH:30]=[C:31]([Cl:36])[CH:32]=4)[CH:27]=3)(=[O:25])=[O:24])[CH2:19][C:18]2=[O:37])[CH2:9][CH2:8][N:7]([C:10]2[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=2)[CH2:6][CH2:5]1.[CH2:38]([O:41][C:42](OC1C=CC([N+]([O-])=O)=CC=1)=[O:43])[CH2:39][CH3:40].C(N(C(C)C)C(C)C)C.C(OCC)(=O)C>CN(C=O)C>[Cl:36][C:31]1[CH:32]=[C:33]2[C:28](=[CH:29][CH:30]=1)[CH:27]=[C:26]([S:23]([N:20]1[CH2:21][CH2:22][N:17]([CH2:16][C:4]3([NH:3][C:42]([O:41][CH2:38][CH2:39][CH3:40])=[O:43])[CH2:9][CH2:8][N:7]([C:10]4[CH:11]=[CH:12][N:13]=[CH:14][CH:15]=4)[CH2:6][CH2:5]3)[C:18](=[O:37])[CH2:19]1)(=[O:24])=[O:25])[CH:35]=[CH:34]2
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 8857Ethyl AcetateHCID 81531DiisopropylethylamineHCID 544839324-Nitrophenyl propyl carbonateHCID 69550750HCID 69550750、化合物

生成物 1

HCID 69550120HCID 69550120、化合物収率 47.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒

実験手順

A solution of 1-[4-amino-1-(4-pyridyl)-4-piperidylmethyl]-4-(6-chloronaphthalene-2-sulfonyl)-2-piperazinone dihydrochloride (235 mg), O-propoxycarbonyl-4-nitrophenol (270 mg) and N-ethyldiisopropylamine (0.348 ml) in DMF (5 ml) was stirred at 80° C. overnight. To the reaction solution was added ethyl acetate, the mixture was washed successively with a 10% aqueous sodium carbonate solution, an aqueous saturated sodium bicarbonate solution and an aqueous saturated sodium chloride solution, dried, and concentrated. The residue was purified by silica gel column chromatography (ethyl acetate:10% aqueous ammonia-containing methanol=90:10→80:20), and crystallized from a mixed solution of acetone and ethyl acetate to obtain the pale brown crystalline title compound (114 mg).

後処理

  1. washthe mixture was washed successively with a 10% aqueous sodium carbonate solution
  2. dry with materialan aqueous saturated sodium bicarbonate solution and an aqueous saturated sodium chloride solution, dried
  3. concentrationconcentrated
  4. customThe residue was purified by silica gel column chromatography (ethyl acetate:10% aqueous ammonia-containing methanol=90:10→80:20)
  5. customcrystallized from a mixed solution of acetone and ethyl acetate

出典と根拠

ORDレコード
ord-0ad99562e80840ca9ad1573722631a80
出典データセット
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07109200B2

反応ノート

読み込み中…

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