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Benzo(d)thiazol-2-amine → (2E)-N-(1,3-benzothiazol-2-yl)-2-cyclopentyloxyimino-2-(4-methylsulfonylphenyl)acetamide

HRID 600977
ノート
印刷プレビュー

反応式

HRID 600977 の反応式
[CH:1]1([O:6]/[N:7]=[C:8](\[C:12]2[CH:17]=[CH:16][C:15]([S:18]([CH3:21])(=[O:20])=[O:19])=[CH:14][CH:13]=2)/[C:9]([OH:11])=O)[CH2:5][CH2:4][CH2:3][CH2:2]1.C(N(CC)C(C)C)(C)C.[NH2:31][C:32]1[S:33][C:34]2[CH:40]=[CH:39][CH:38]=[CH:37][C:35]=2[N:36]=1>C(Cl)Cl>[S:33]1[C:34]2[CH:40]=[CH:39][CH:38]=[CH:37][C:35]=2[N:36]=[C:32]1[NH:31][C:9](=[O:11])/[C:8](=[N:7]/[O:6][CH:1]1[CH2:2][CH2:3][CH2:4][CH2:5]1)/[C:12]1[CH:17]=[CH:16][C:15]([S:18]([CH3:21])(=[O:20])=[O:19])=[CH:14][CH:13]=1
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

5

反応物 3

HCID 8706Benzo(d)thiazol-2-amineHCID 81531DiisopropylethylamineHCID 57630055HCID 57630055、化合物

生成物 1

HCID 24990022(2E)-N-(1,3-benzothiazol-2-yl)-2-cyclopentyloxyimino-2-(4-methylsulfonylphenyl)acetamide収率 63.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

(E)-Cyclopentyloxyimino-(4-methanesulfonyl-phenyl)-acetic acid (37 mg, 0.12 mmol), N,N-diisopropylethylamine (92 μL, 0.53 mmol) and 2-aminobenzothiazole (27 mg, 0.18 mmol) were combined in methylene chloride (2 mL) and cooled to 0° C. O-(7-Azabenzotriazole-1-yl)-N,N,N′N′-tetramethyluronium hexafluorophosphate (67 mg, 0.18 mmol) was added and the cooling bath was removed. After stirring 16 h, the reaction mixture was diluted with chloroform (2 mL) and washed with saturated aqueous sodium bicarbonate solution (1.5 mL). The aqueous phase was extracted with chloroform (1.5 mL) and the combined organic phases were filtered through sodium sulfate and evaporated in vacuo. The residue was purified by flash column chromatography (Merck silica gel 60, 40-63 μm; 40% ethyl acetate/hexanes) to afford (E)-N-benzothiazol-2-yl-2-cyclopentyloxyimino-2-(4-methanesulfonyl-phenyl)-acetamide (34 mg, 43%) as a white solid: LC-MS (ESI) m/e calcd for C21H21N3O4S2 [M+] 443.10, found 444 [M+H+]; H1-NMR (400 MHz, CDCl3) δ ppm 1.66 (m, 4 H, 2×CH2), 1.90 (m, 4 H, 2×CH2), 3.11 (s, 3 H, SO2CH3), 4.95 (m, 1 H, OCH), 7.35 (brt, 1 H, Ar), 7.48 (brt, 1 H, Ar), 7.72 (d, J=8.4 Hz, 2 H, Ar), 7.83 (m, 2H, Ar), 8.03 (d, J=8.4 Hz, 2 H, Ar), 10.24 (s, 1 H, NH).

後処理

  1. customthe cooling bath was removed
  2. additionthe reaction mixture was diluted with chloroform (2 mL)
  3. washwashed with saturated aqueous sodium bicarbonate solution (1.5 mL)
  4. extractionThe aqueous phase was extracted with chloroform (1.5 mL)
  5. filtrationthe combined organic phases were filtered through sodium sulfate
  6. customevaporated in vacuo
  7. customThe residue was purified by flash column chromatography (Merck silica gel 60, 40-63 μm; 40% ethyl acetate/hexanes)

出典と根拠

ORDレコード
ord-c30da581484846b5b77fce67e5484036
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07902248B2

反応ノート

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