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Potassium Carbonate → 3-[6-Amino-5-(1,3-benzothiazol-2-yl)pyridin-3-yl]phenol

HRID 1926371
ノート
印刷プレビュー

反応式

HRID 1926371 の反応式
[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[C:10]1[C:11]([NH2:17])=[N:12][CH:13]=[C:14](Br)[CH:15]=1.[OH:18][C:19]1[CH:20]=[C:21](B(O)O)[CH:22]=[CH:23][CH:24]=1.C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1.O.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[NH2:17][C:11]1[N:12]=[CH:13][C:14]([C:23]2[CH:24]=[C:19]([OH:18])[CH:20]=[CH:21][CH:22]=2)=[CH:15][C:10]=1[C:2]1[S:1][C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=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 11430Potassium CarbonateHCID 2734359(3-hydroxyphenyl)boronic AcidHCID 67389127HCID 67389127、化合物

生成物 1

HCID 675207593-[6-Amino-5-(1,3-benzothiazol-2-yl)pyridin-3-yl]phenol

試薬・触媒・溶媒 3

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)触媒
HCID 962
Water
溶媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

A mixture of 3-benzothiazol-2-yl-5-bromopyridin-2-ylamine (BB7) (100 mg, 0.330 mmol), 3-hydroxyphenylboronic acid (68 mg, 0.49 mmol) and potassium carbonate (140 mg, 0.980 mmol) in 1,4-dioxane (4.5 mL) and H2O (1.5 mL) was degassed and refilled with argon (3×) prior to the addition of Pd(dppf)Cl2 (10 mg, 0.020 mmol). The reaction mixture was degassed and refilled with argon (2×) and left to stir at 100° C. for 30 min in the microwave reactor. Then, the mixture was passed through a pad of Celite and to the filtrate was partitioned between EtOAc and NaHCO3 aq. soln. (3×). The combined organic extracts were treated with brine, dried over anhydrous Na2SO4, filtered, and concentrated in vacuo. Purification via silica gel chromatography (5% MeOH in DCM) afforded the title compound as a yellow solid. 1H NMR (400 MHz, DMSO-d6): δ=6.75-6.77 (m, 1H), 7.04-7.04 (m, 1H), 7.10-7.12 (m, 1H), 7.27 (t, J=8.0 Hz, 1H), 7.46-7.50 (m, 1H), 7.55-7.58 (m, 1H), 8.02 (br.s, 2H), 8.10-8.16 (m, 3H), 8.46 (d, J=4.0 Hz, 1H), 9.54 (s, 1H). MS (ES+): m/z=320.09 (100) [MH+]. HPLC: tR=3.44 min (ZQ3, polar—5 min).

後処理

  1. customwas degassed
  2. additionrefilled with argon (3×)
  3. customThe reaction mixture was degassed
  4. additionrefilled with argon (2×)
  5. waitleft
  6. customwas partitioned between EtOAc and NaHCO3 aq. soln
  7. additionThe combined organic extracts were treated with brine
  8. dry with materialdried over anhydrous Na2SO4
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo
  11. customPurification via silica gel chromatography (5% MeOH in DCM)

出典と根拠

ORDレコード
ord-fc6c0a8950e0473fbdb42b6d397002f1
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08178668B2

反応ノート

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