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Sodium Hydroxide → HCID 66775751、化合物

HRID 1644848
ノート
印刷プレビュー

反応式

HRID 1644848 の反応式
[CH2:1]([C:5]1[S:9][C:8]([S:10]([NH:13][C:14]([CH3:17])([CH3:16])[CH3:15])(=[O:12])=[O:11])=[C:7](B(O)O)[CH:6]=1)[CH:2]([CH3:4])[CH3:3].Br[C:22]1[CH:33]=[CH:32][C:25]([CH2:26][N:27]2[CH:31]=[N:30][CH:29]=[N:28]2)=[CH:24][CH:23]=1.[OH-].[Na+]>C1(C)C=CC=CC=1.C(O)C.CC([O-])=O.CC([O-])=O.[Pd+2].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[N:27]1([CH2:26][C:25]2[CH:24]=[CH:23][C:22]([C:7]3[CH:6]=[C:5]([CH2:1][CH:2]([CH3:4])[CH3:3])[S:9][C:8]=3[S:10]([NH:13][C:14]([CH3:17])([CH3:16])[CH3:15])(=[O:12])=[O:11])=[CH:33][CH:32]=2)[CH:31]=[N:30][CH:29]=[N:28]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 3

HCID 14798Sodium HydroxideHCID 11484000(2-(N-(tert-Butyl)sulfamoyl)-5-isobutylthiophen-3-yl)boronic acidHCID 19043019HCID 19043019、化合物

生成物 1

HCID 66775751HCID 66775751、化合物収率 66.6%

試薬・触媒・溶媒 3

HCID 11776Triphenylphosphine触媒
HCID 167845
palladium(II) acetate
触媒
HCID 21863594Toluene ethanol溶媒

反応条件

温度
80 °C

実験手順

5-iso-Butyl-2-(N-tert-butylaminosulfonyl)thiophene-3-boronic acid (0.479 g, 1.5 mmol, see Example 1(c) above), 1-(4-bromobenzyl)-1H-[1,2,4]triazole (0.238 g, 1 mmol, see step (a) above), Pd(OAc)2 (15.7 mg, 0.03 mmol), triphenyl phosphine (15.7 mg, 0.06 mmol) and NaOH (0.16 g, 4 mmol) were dissolved in 4 mL of toluene/ethanol (4:1) in a thick walled glass tube, and were then heated to 80° C. for 1 h. The reaction mixture was cooled to rt, extracted with ethyl acetate and water and subsequently dried over K2CO3. The solvent was evaporated and the reaction mixture was separated on a silica column (dichloromethane+1% methanol to dichloromethane+4% methanol) to yield 0.288 g of the sub-title compound (65% yield).

後処理

  1. temperatureThe reaction mixture was cooled to rt
  2. extractionextracted with ethyl acetate and water
  3. dry with materialsubsequently dried over K2CO3
  4. customThe solvent was evaporated
  5. customthe reaction mixture was separated on a silica column (dichloromethane+1% methanol to dichloromethane+4% methanol)

出典と根拠

ORDレコード
ord-cba9a1596d27426a9525a18b2923a596
出典データセット
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08124638B2

反応ノート

読み込み中…

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