Sodium Carbonate → HCID 68839429、化合物

HRID 660730ノート

反応式

HRID 660730 の反応式
[CH2:1]([O:8][C:9]1[CH:14]=[C:13](I)[CH:12]=[CH:11][C:10]=1[N:16]1[S:20](=[O:22])(=[O:21])[NH:19][C:18](=[O:23])[CH2:17]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:24]([Si:27]([CH:39]([CH3:41])[CH3:40])([CH:36]([CH3:38])[CH3:37])[N:28]1[CH:32]=[CH:31][C:30](B(O)O)=[CH:29]1)([CH3:26])[CH3:25].C([O-])([O-])=O.[Na+].[Na+]>COCCOC.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>[CH2:1]([O:8][C:9]1[CH:14]=[C:13]([C:30]2[CH:31]=[CH:32][N:28]([Si:27]([CH:36]([CH3:38])[CH3:37])([CH:39]([CH3:41])[CH3:40])[CH:24]([CH3:25])[CH3:26])[CH:29]=2)[CH:12]=[CH:11][C:10]=1[N:16]1[S:20](=[O:22])(=[O:21])[NH:19][C:18](=[O:23])[CH2:17]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 3

HCID 10340Sodium CarbonateHCID 27633031-(Triisopropylsilyl)pyrrole-3-boronic acidHCID 688386435-(2-Benzyloxy-4-iodophenyl)-1,1-dioxo-1,2,5-thiadiazolidin-3-one

生成物 1

HCID 68839429HCID 68839429、化合物

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
120 °C

実験手順

To a solution of 5-(2-benzyloxy-4-iodophenyl)-1,1-dioxo-1,2,5-thiadiazolidin-3-one (100 mg, 0.225 mmol) in DME (5 mL) is added 1-triisopropylsilylpyrrole-3-boronic acid (120 mg, 0.450 mmol), Pd(PPh3)4 (27 mg, 0.023 mmol) and 0.5 mL of Na2CO3 (2M aqueous solution) and the mixture is heated in a microwave apparatus at 120° C. for 5 min. The mixture is concentrated under reduced pressure and the residue purified by reverse phase MPLC using a gradient of 10-50% MeCN/water as eluent to afford the title compound: (M−1)−=538.

後処理

  1. concentrationThe mixture is concentrated under reduced pressure
  2. customthe residue purified by reverse phase MPLC

出典と根拠

ORDレコード
ord-5af0f2be0f7847ddb8a0b6853568e1d2
出典データセット
uspto-grants-2011_12
特許番号
US08084448B2

反応ノート

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