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Isobutanol → 3-[4-(4-Cyano-3-fluoro-phenyl)-piperazine-1-carbonyl]-4-isobutoxy-benzenesulfonamide

HRID 1820826
ノート
印刷プレビュー

反応式

HRID 1820826 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:14][CH2:13][N:12]([C:15]([C:17]3[CH:18]=[C:19]([S:24]([NH2:27])(=[O:26])=[O:25])[CH:20]=[CH:21][C:22]=3[OH:23])=[O:16])[CH2:11][CH2:10]2)=[CH:5][C:4]=1[F:28])#[N:2].[CH3:29][CH:30]([CH3:33])[CH2:31]O.C1(P(C2C=CC=CC=2)C2C=CC=CN=2)C=CC=CC=1.N(C(OC(C)(C)C)=O)=NC(OC(C)(C)C)=O>C1COCC1.C(OCC)(=O)C>[C:1]([C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:10][CH2:11][N:12]([C:15]([C:17]3[CH:18]=[C:19]([S:24]([NH2:27])(=[O:25])=[O:26])[CH:20]=[CH:21][C:22]=3[O:23][CH2:29][CH:30]([CH3:33])[CH3:31])=[O:16])[CH2:13][CH2:14]2)=[CH:5][C:4]=1[F:28])#[N: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

7

反応物 4

HCID 6560IsobutanolHCID 97268Di-tert-butyl azodicarboxylateHCID 6218932-PyridyldiphenylphosphineHCID 690384423-[4-(4-Cyano-3-fluoro-phenyl)-piperazine-1-carbonyl]-4-hydroxy-benzenesulfonamide2 回

生成物 1

HCID 690383983-[4-(4-Cyano-3-fluoro-phenyl)-piperazine-1-carbonyl]-4-isobutoxy-benzenesulfonamide

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
60 °C

実験手順

To 0.1 mmol (3-[4-(4-cyano-3-fluoro-phenyl)-piperazine-1-carbonyl]-4-hydroxy-benzenesulfonamide (compound 6.38), 0.5 mmol 2-methyl-1-propanol and 0.3 mmol diphenyl-2-pyridylphosphine in 4 ml THF was added 0.3 mmol di-tert-butyl azodicarboxylate, and the mixture was stirred at 60° C. for 4 h. The mixture was then diluted with ethyl acetate and washed twice with 5 M aq HCl and then with saturated aq NaCl solution. The organic phase was then dried with Na2SO4, and concentrated in vacuo. The residue was triturated in ether to afford the title compound. MS (m/e): 459.2 ([M−H]−, 100%)

後処理

  1. washwashed twice with 5 M aq HCl
  2. dry with materialThe organic phase was then dried with Na2SO4
  3. concentrationconcentrated in vacuo
  4. customThe residue was triturated in ether

出典と根拠

ORDレコード
ord-9a98615c005047058469ce294c529fdf
出典データセット
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07605163B2

反応ノート

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