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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Water → HCID 86653304、化合物

HRID 1695746
ノート
印刷プレビュー

反応式

HRID 1695746 の反応式
Br[C:2]1[CH:3]=[C:4]([NH2:12])[C:5]2[CH:6]=[N:7][N:8]([CH3:11])[C:9]=2[CH:10]=1.C(=O)([O-])[O-].[Na+].[Na+].[Cl:19][C:20]1[N:25]=[CH:24][C:23](B(O)O)=[CH:22][C:21]=1[NH:29][S:30]([CH3:33])(=[O:32])=[O:31].O>O1CCOCC1.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]>[NH2:12][C:4]1[CH:3]=[C:2]([C:23]2[CH:22]=[C:21]([NH:29][S:30]([CH3:33])(=[O:32])=[O:31])[C:20]([Cl:19])=[N:25][CH:24]=2)[CH:10]=[C:9]2[C:5]=1[CH:6]=[N:7][N:8]2[CH3:11]
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 10340Sodium CarbonateHCID 582557716-Bromo-1-methyl-1h-indazol-4-amineHCID 86653303{6-Chloro-5-[(methylsulfonyl)amino]-3-pyridinyl}boronic acid

生成物 1

HCID 86653304HCID 86653304、化合物収率 29.9%

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
120 °C

実験手順

6-Bromo-1-methyl-1H-indazol-4-amine (340 mg), sodium carbonate (638 mg) and Pd(dppf)Cl2 (110 mg) were weighed to a 10-20 ml microwave vial. {6-Chloro-5-[(methylsulfonyl)amino]-3-pyridinyl}boronic acid (377 mg) dissolved in 1,4-dioxane (6 ml) was added followed by water (6 ml). The reaction was heated for 15 min at 120° C. in the microwave. The reaction was passed through a 2 g silica cartridge, washing with methanol. The solvent was evaporated under nitrogen blow down. The residue was purified on the ISCO companion using a 40 g silica cartridge and a gradient of 2-8% methanol in DCM (containing 1% ammonia) over 15 mins at 40 ml/min. Product-containing fractions were combined and dried down to give title compound (158 mg).

後処理

  1. additionwas added
  2. washwashing with methanol
  3. customThe solvent was evaporated under nitrogen blow down
  4. customThe residue was purified on the ISCO companion
  5. customdried down

出典と根拠

ORDレコード
ord-96256255827443ccadac58741674420a
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08163743B2

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