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Sodium Bicarbonate → HCID 89782936、化合物

HRID 58105
ノート
印刷プレビュー

反応式

HRID 58105 の反応式
CC1(C)C(C)(C)OB([C:9]2[CH:17]=[C:16]([C:18]([F:21])([F:20])[F:19])[CH:15]=[C:14]3[C:10]=2[CH:11]=[N:12][NH:13]3)O1.Br[C:24]1[CH:25]=[CH:26][C:27]([S:30]([NH:33][CH2:34][CH2:35][OH:36])(=[O:32])=[O:31])=[N:28][CH:29]=1.[C:37](=[O:40])(O)[O-:38].[Na+]>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].O1CCOCC1>[C:37]([OH:38])([C:18]([F:21])([F:20])[F:19])=[O:40].[OH:36][CH2:35][CH2:34][NH:33][S:30]([C:27]1[CH:26]=[CH:25][C:24]([C:9]2[CH:17]=[C:16]([C:18]([F:19])([F:20])[F:21])[CH:15]=[C:14]3[C:10]=2[CH:11]=[N:12][NH:13]3)=[CH:29][N:28]=1)(=[O:32])=[O:31]
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 516892Sodium BicarbonateHCID 59406275HCID 59406275、化合物HCID 897828064-(Tetramethyl-1,3,2-dioxaborolan-2-yl)-6-(trifluoromethyl)-1H-indazole

生成物 2

HCID 6422Trifluoroacetic acidHCID 89782936HCID 89782936、化合物収率 66.3%

試薬・触媒・溶媒 2

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

反応条件

温度
140 °C

実験手順

4-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)-6-(trifluoromethyl)-1H-indazole (40 mg, 0.128 mmol), 5-bromo-N-(2-hydroxyethyl)pyridine-2-sulfonamide (43.2 mg, 0.154 mmol), PdCl2(dppf) (9.38 mg, 0.013 mmol), sodium bicarbonate (0.274 mL, 0.513 mmol), and dioxane (2 mL) were mixed in a 10 mL vial to give an orange suspension. The vial was sealed and then heated to 140° C. for 20 minutes in a microwave reactor. The reaction mixture was subsequently filtered and the product was purified by preparative HPLC, eluting with a gradient of 25-50% ACN (containing 0.035% TFA) in H2O (containing 0.05% TFA). The pure fractions were lyophilized to give a TFA salt of the title compound as a white solid (16.4 mg, 25.6%). 1H NMR (400 MHz, DMSO-d6) δ ppm 3.05 (q, J=6.48 Hz, 2H), 3.40-3.46 (m, 7H), 7.70 (d, J=1.01 Hz, 1H), 7.96 (t, J=5.81 Hz, 1H), 8.08 (dd, J=8.21, 0.88 Hz, 2H), 8.45 (s, 1H), 8.51 (dd, J=8.21, 2.40 Hz, 1H), 9.15 (dd, J=2.27, 1.01 Hz, 1H); ESI-MS m/z [M+H]+ calc'd for C15H13F3N4O3S, 387.1. found 387.2.

後処理

  1. customto give an orange suspension
  2. customThe vial was sealed
  3. filtrationThe reaction mixture was subsequently filtered
  4. customthe product was purified by preparative HPLC
  5. washeluting with a gradient of 25-50% ACN (containing 0.035% TFA) in H2O (containing 0.05% TFA)

出典と根拠

ORDレコード
ord-0ddaf83dd57d4548ad7eaed76e6c9aae
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09434743B2

反応ノート

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