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Water → 5-(6-chloro-3-methylpyridin-2-yl)-1-methyl-1H-indazole

HRID 879560
ノート
印刷プレビュー

反応式

HRID 879560 の反応式
[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][C:7](B(O)O)=[CH:8][CH:9]=2)[CH:4]=[N:3]1.Br[C:15]1[C:20]([CH3:21])=[CH:19][CH:18]=[C:17]([Cl:22])[N:16]=1.O.C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[Cl:22][C:17]1[N:16]=[C:15]([C:7]2[CH:6]=[C:5]3[C:10](=[CH:9][CH:8]=2)[N:2]([CH3:1])[N:3]=[CH:4]3)[C:20]([CH3:21])=[CH:19][CH:18]=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 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 225589101-Methyl-1H-indazole-5-boronic acidHCID 534166752-Bromo-6-chloro-3-methylpyridine

生成物 1

HCID 867003845-(6-chloro-3-methylpyridin-2-yl)-1-methyl-1H-indazole

試薬・触媒・溶媒 2

HCID 178418397
HCID 178418397、化合物
触媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
110 °C

実験手順

In a 10 mL reaction vial, the 1-methyl-1H-indazol-5-ylboronic acid (500 mg, 2.84 mmol) and the 2-bromo-6-chloro-3-methylpyridine (585 mg, 2.84 mmol) were dissolved in dioxane (7 mL) and water (1.7 mL) under argon atmosphere. The mixture was bubbled with argon for 5 min. Then potassium carbonate (979 mg, 7.1 mmol) and Pd(PPh3)4 (49 3 mg, 0.428 mmol) were added sequentially. The resulting reaction mixture was then sealed and heated in oil bath at 110° C. for 2.5 h. Reaction was then partitioned between EtOAc (30 mL) and water (30 mL).The organic phase was washed with water (3×20 mL) and was concentrated. Residue was purified on silica gel column with 0-50% EtOAc/Hex to afford the title compound. LCMS-ESI+: calc'd for: C14H12ClN3: 258.1 and 260.1 (M+H+); found: 258.0 and 260.0 (M+H+).

後処理

  1. customIn a 10 mL reaction vial
  2. customThe mixture was bubbled with argon for 5 min
  3. customThe resulting reaction mixture
  4. customwas then sealed
  5. customReaction
  6. customwas then partitioned between EtOAc (30 mL) and water (30 mL).The organic phase
  7. washwas washed with water (3×20 mL)
  8. concentrationwas concentrated
  9. customResidue was purified on silica gel column with 0-50% EtOAc/Hex

出典と根拠

ORDレコード
ord-b5c872eeb1ad4bcfadee83c0d521edbd
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08987250B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート