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Water → HCID 73775993、化合物

HRID 2207277
ノート
印刷プレビュー

反応式

HRID 2207277 の反応式
[C:1]([C:3]1[CH:4]=[C:5]([S:23]([NH:26][C:27]2[S:28][CH:29]=[CH:30][N:31]=2)(=[O:25])=[O:24])[CH:6]=[CH:7][C:8]=1[O:9][C:10]1[CH:11]=[N:12][C:13]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[CH:14][C:15]=1I)#[N:2].[F:32][C:33]1[C:38](B(O)O)=[CH:37][CH:36]=[CH:35][N:34]=1.C([O-])([O-])=O.[Na+].[Na+].O>CN(C)C=O.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>[C:1]([C:3]1[CH:4]=[C:5]([S:23]([NH:26][C:27]2[S:28][CH:29]=[CH:30][N:31]=2)(=[O:25])=[O:24])[CH:6]=[CH:7][C:8]=1[O:9][C:10]1[CH:11]=[N:12][C:13]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[CH:14][C:15]=1[C:38]1[C:33]([F:32])=[N:34][CH:35]=[CH:36][CH:37]=1)#[N:2]
参加物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 10340Sodium CarbonateHCID 27832702-Fluoropyridine-3-boronic acidHCID 90100535HCID 90100535、化合物

生成物 1

HCID 73775993HCID 73775993、化合物収率 30%

試薬・触媒・溶媒 2

HCID 178418397
HCID 178418397、化合物
触媒
HCID 6228Dimethylformamide溶媒

実験手順

10 mg (0.02 mmol) of 3-cyano-4-((4-iodo-6-phenylpyridin-3-yl)oxy)-N-(thiazol-2-yl)benzenesulfonamide was dissolved in 3 mL of N,N-dimethylformamide, and 3.7 mg (0.03 mmol) of (2-fluoropyridin-3-yl)boronic acid was added thereto, and then 2.0 mg (10 mol %) of Pd(PPh3)4, 5.6 mg (0.6 mmol) of Na2CO3, and 1 mL of H2O were added thereto. After reacting with microwave reactor at 120° C. for 5 minutes, the solvent was removed, and the remaining material was diluted with ethyl acetate and the organic layer was separated, and washed with saturated sodium chloride. The organic layer was collected, dried with magnesium sulfate to remove water, and concentrated under reduced pressure, and the residue was purified by column chromatography (developing solvent, hexane:ethyl acetate=3:1) to obtain 3 mg (30% yield) of the title compound.

後処理

  1. customthe solvent was removed
  2. additionthe remaining material was diluted with ethyl acetate
  3. customthe organic layer was separated
  4. washwashed with saturated sodium chloride
  5. customThe organic layer was collected
  6. dry with materialdried with magnesium sulfate
  7. customto remove water
  8. concentrationconcentrated under reduced pressure
  9. customthe residue was purified by column chromatography (developing solvent, hexane:ethyl acetate=3:1)

出典と根拠

ORDレコード
ord-013606f062c3405cb7f9500aad82430c
出典データセット
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09376429B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート