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Acetic Anhydride → HCID 68421046、化合物

HRID 1817115
ノート
印刷プレビュー

反応式

HRID 1817115 の反応式
[CH2:1]([O:3][C:4](=[O:24])[C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12]2[N:16]=[CH:15][N:14]([C:17]3[CH:22]=[CH:21][N:20]=[C:19](Cl)[CH:18]=3)[N:13]=2)=[CH:7][CH:6]=1)[CH3:2].[CH3:25][C@H:26]1[NH:31][C@@H:30]([CH3:32])[CH2:29][NH:28][CH2:27]1.CCN(C(C)C)C(C)C.[C:42](OC(=O)C)(=[O:44])[CH3:43]>CN1C(=O)CCC1.C(Cl)Cl.CN(C=O)C>[CH2:1]([O:3][C:4](=[O:24])[C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12]2[N:16]=[CH:15][N:14]([C:17]3[CH:22]=[CH:21][N:20]=[C:19]([N:28]4[CH2:29][CH:30]([CH3:32])[N:31]([C:42](=[O:44])[CH3:43])[CH:26]([CH3:25])[CH2:27]4)[CH:18]=3)[N:13]=2)=[CH:7][CH:6]=1)[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 7918Acetic AnhydrideHCID 81531DiisopropylethylamineHCID 6950261rel-(2R,6S)-2,6-dimethylpiperazineHCID 58883268HCID 58883268、化合物

生成物 1

HCID 68421046HCID 68421046、化合物収率 44%

試薬・触媒・溶媒 3

HCID 6228Dimethylformamide
溶媒
HCID 6344Dichloromethane溶媒
HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
250 °C

実験手順

To a solution of 500 mg of 4-[1-(2-Chloro-pyridin-4-yl)-1H-[1,2,4]triazol-3-ylamino]-benzoic acid ethyl ester (1.45 mMol, 1 equiv) in 10 mL of NMP was added 400 mg of cis-3,5 dimethyl piperazine (3.50 mMol, 2.41 equiv). The stirred solution was heated to 250° C. via microwave irradiation for 15 min. The crude product was precipitated by pouring into 100 mL of water and isolated by filtration. The crude product was then redissolved in 10 mL of CH2Cl2 and 2 mL of DMF. To the stirred solution was added sequentially 1 mL of Hunig's base and 500 μL of acetic anhydride. After 3 hr at 25° C., the reaction mixture was concentrated to a dark oil and purified by flash chromatography (10:1 CH2Cl2:MeOH), yielding 300 mg of 4-{1-[2-(4-Acetyl-3,5-dimethyl-piperazin-1-yl)-pyridin-4-yl]-1H-[1,2,4]triazol-3-ylamino}-benzoic acid ethyl ester (0.647 mMol, 44% yield) as a white solid. 1H NMR (500 MHz, CDCl3) ∂ 8.44 (1H, s), 8.22 (1H, d), 8.05 (2H, d), 7.61 (3H, m), 7.27 (1H, s), 7.02 (1H, s), 6.86 (1H, d), 4.40 (2H, q), 3.50 (2H, q), 3.40 (2H, m), 3.20 (2H, m), 2.20 (3H, s), 1.40 (6H, m), 1.20 (3H, t) ppm. LC/MS: 2.68 min/464 (M+1).

後処理

  1. customThe crude product was precipitated
  2. additionby pouring into 100 mL of water
  3. customisolated by filtration
  4. concentrationthe reaction mixture was concentrated to a dark oil
  5. custompurified by flash chromatography (10:1 CH2Cl2:MeOH)

出典と根拠

ORDレコード
ord-bb54ede0c62c4a42bbc8911c1bc087ff
出典データセット
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07598245B2

反応ノート

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