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1-Methylpiperazine → HCID 131723007、化合物

HRID 2268534
ノート
印刷プレビュー

反応式

HRID 2268534 の反応式
[CH3:1][O:2][C:3]1[C:4](=[O:29])[C:5]2[CH2:6][CH:7]([CH2:15][CH2:16][CH2:17][CH2:18][O:19][C:20]3[CH:28]=[CH:27][C:23]([C:24]([OH:26])=O)=[CH:22][CH:21]=3)[CH2:8][C:9]=2[C:10](=[O:14])[C:11]=1[O:12][CH3:13].[CH3:30][N:31]1[CH2:36][CH2:35][NH:34][CH2:33][CH2:32]1.Cl.C(N=C=NCCCN(C)C)C.O.ON1C2C=CC=CC=2N=N1>O.C(N(CC)CC)C>[CH3:13][O:12][C:11]1[C:10](=[O:14])[C:9]2[CH2:8][CH:7]([CH2:15][CH2:16][CH2:17][CH2:18][O:19][C:20]3[CH:21]=[CH:22][C:23]([C:24]([N:34]4[CH2:35][CH2:36][N:31]([CH3:30])[CH2:32][CH2:33]4)=[O:26])=[CH:27][CH:28]=3)[CH2:6][C:5]=2[C:4](=[O:29])[C:3]=1[O:2][CH3:1]
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 4

HCID 531671-MethylpiperazineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 18348629HCID 18348629、化合物

生成物 1

HCID 131723007HCID 131723007、化合物収率 49.3%

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 8471Triethylamine溶媒

実験手順

A mixture of 4-[4-(5,6-dimethoxy-4,7-dioxoindan-2-yl)butoxy]benzoic acid (500 mg), 1-methylpiperazine (250 mg), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (479 mg), 1-hydroxybenzotriazole monohydrate (383 mg), triethylamine (0.697 ml), andTHF (20 ml) was stirred at room temperature for 10 hr. The reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride and dried. The solvent was removed in vacuo. The residue was purified by alumina column chromatography (ethyl acetate) and then with recrystallization from ethyl acetate-diisopropylether to yield the entitled compound (297 mg) as crystals.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with water and saturated aqueous sodium chloride
  3. customdried
  4. customThe solvent was removed in vacuo
  5. customThe residue was purified by alumina column chromatography (ethyl acetate)
  6. customwith recrystallization from ethyl acetate-diisopropylether

出典と根拠

ORDレコード
ord-8c8bbb5bd7884fa8863c763204db3211
出典データセット
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06326369B1

反応ノート

読み込み中…

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