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Sodium Carbonate → N-(6-(2-(4-methoxyphenylsulfonyl)thiazol-5-yl)benzo[d]thiazol-2-yl)acetamide

HRID 2077496
ノート
印刷プレビュー

反応式

HRID 2077496 の反応式
Br[C:2]1[S:6][C:5]([S:7]([C:10]2[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[CH:12][CH:11]=2)(=[O:9])=[O:8])=[N:4][CH:3]=1.CC1(C)C(C)(C)OB([C:26]2[CH:38]=[CH:37][C:29]3[N:30]=[C:31]([NH:33][C:34](=[O:36])[CH3:35])[S:32][C:28]=3[CH:27]=2)O1.C(=O)([O-])[O-].[Na+].[Na+]>O1CCOCC1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Pd]>[CH3:17][O:16][C:13]1[CH:14]=[CH:15][C:10]([S:7]([C:5]2[S:6][C:2]([C:26]3[CH:38]=[CH:37][C:29]4[N:30]=[C:31]([NH:33][C:34](=[O:36])[CH3:35])[S:32][C:28]=4[CH:27]=3)=[CH:3][N:4]=2)(=[O:9])=[O:8])=[CH:11][CH:12]=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

7

反応物 3

HCID 10340Sodium CarbonateHCID 51354026n-(6-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)benzo[d]thiazol-2-yl)acetamideHCID 575851575-Bromo-2-(4-methoxyphenylsulfonyl)thiazole

生成物 1

HCID 25183186N-(6-(2-(4-methoxyphenylsulfonyl)thiazol-5-yl)benzo[d]thiazol-2-yl)acetamide

試薬・触媒・溶媒 3

HCID 11979704
Tetrakis(triphenylphosphine)palladium
触媒
HCID 178418397HCID 178418397、化合物触媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
80 °C

実験手順

5-Bromo-2-(4-methoxyphenylsulfonyl)thiazole (134.8 mg, 4.034 mmol), N-(6-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzo[d]thiazol-2-yl)acetamide (163.6 mg, 0.5141 mmol), sodium carbonate (0.40 mL, 2.0 M in water, 0.80 mmol), and palladiumtetrakis(triphenyl phosphine) (59.5 mg, 51.5 μmol) were suspended in 1,4-dioxane (3.2 mL) and the reaction mixture was stirred and heated at 80° C. for 1.5 hours. Additional Pd(PPh3)4 (78 mg) was added to the mixture and stirring and heating were continued at 90° C. for another 90 minutes, at which time the reaction was cooled to RT. The organic phase was decanted, and the residual solid was washed with DCM and MeOH and filtered through a Celite® (diatomaceous earth) pad. This pad was washed with DCM and MeOH, and the filtrate was combined with the decanted suspension and concentrated. The solid was treated with Et2O and filtered. Solid washed with Et2O and purified on HPLC (10% to 95% MeCN/water with 0.1% TFA over 40 minutes) to afford N-(6-(2-(4-methoxyphenylsulfonyl)thiazol-5-yl)benzo[d]thiazol-2-yl)acetamide. MS (ESI pos. ion) m/z: 446. Calculated exact mass for C19H15N3O4S3: 445. 1H NMR (400 MHz, DMSO-d6): 12.51 (s, 1H), 8.48 (s, 1H), 8.45 (s, 1H), 7.99 (d, J=9.0 Hz, 2H), 7.81 (m, 2H), 7.22 (d, J=8.5 Hz, 2H), 3.87 (s, 3H), 2.22 (s, 3H).

後処理

  1. stirringstirring
  2. temperatureheating
  3. temperaturethe reaction was cooled to RT
  4. customThe organic phase was decanted
  5. washthe residual solid was washed with DCM and MeOH
  6. filtrationfiltered through a Celite® (diatomaceous earth) pad
  7. washThis pad was washed with DCM and MeOH
  8. concentrationconcentrated
  9. additionThe solid was treated with Et2O
  10. filtrationfiltered
  11. washSolid washed with Et2O
  12. custompurified on HPLC (10% to 95% MeCN/water with 0.1% TFA over 40 minutes)

出典と根拠

ORDレコード
ord-ae6a6842a8c24623beab1e3f484ce3be
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07928140B2

反応ノート

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