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Sodium Hydroxide → 3-[3-(2-Phenylimidazol-1-ylmethyl)phenyl]-5-iso-butyl-N-tert-butylthiophene-2-sulfonamide

HRID 659689
ノート
印刷プレビュー

反応式

HRID 659689 の反応式
Br[C:2]1[N:3]([CH2:7][C:8]2[CH:9]=[C:10]([C:14]3[CH:18]=[C:17]([CH2:19][CH:20]([CH3:22])[CH3:21])[S:16][C:15]=3[S:23]([NH:26][C:27]([CH3:30])([CH3:29])[CH3:28])(=[O:25])=[O:24])[CH:11]=[CH:12][CH:13]=2)[CH:4]=[CH:5][N:6]=1.[C:31]1(B(O)O)[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1.[OH-].[Na+]>C1(C)C=CC=CC=1.C(O)C.CCOC(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:31]1([C:2]2[N:3]([CH2:7][C:8]3[CH:9]=[C:10]([C:14]4[CH:18]=[C:17]([CH2:19][CH:20]([CH3:22])[CH3:21])[S:16][C:15]=4[S:23]([NH:26][C:27]([CH3:30])([CH3:29])[CH3:28])(=[O:25])=[O:24])[CH:11]=[CH:12][CH:13]=3)[CH:4]=[CH:5][N:6]=2)[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=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

8

反応物 3

HCID 14798Sodium HydroxideHCID 66827Phenylboronic Acid2 回HCID 671329713-[3-(2-bromoimidazol-1-ylmethyl)phenyl]-5-iso-butyl-N-tert-butylthiophene-2-sulfonamide

生成物 1

HCID 671328543-[3-(2-Phenylimidazol-1-ylmethyl)phenyl]-5-iso-butyl-N-tert-butylthiophene-2-sulfonamide収率 49%

試薬・触媒・溶媒 4

HCID 178418397
HCID 178418397、化合物
触媒
2 回
HCID 702Ethanol溶媒
HCID 1140Toluene溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
90 °C

実験手順

To a solution of 3-[3-(2-bromoimidazol-1-ylmethyl)phenyl]-5-iso-butyl-N-tert-butylthiophene-2-sulfonamide (58.5 mg, 0.115 mmol; see Example 11(b)) in toluene (5 mL) and ethanol (0.5 mL) was added phenyl boronic acid (55.9 mg, 0.458 mmol), Pd(PPh3)4 (7.9 mg, 6.88 μmol), NaOH (0.46 mL, 0.688 mmol, 1.5 M aq), and the reaction mixture was stirred for 4 h at 90° C. Another portion of phenyl boronic acid (20.0 mg, 0.164 mmol) and Pd(PPh3)4 (2.0 mg, 1.7 μmol) were added and the reaction was stirred overnight at 90° C. The reaction mixture was diluted with EtOAc (30 mL) and washed with water, dried (over anhydrous MgSO4), concentrated in vacuo, and the residue purified by flash chromatography using EtOAc:hexane (8:2) as eluent to give the sub-title compound in 49% yield (28.4 mg, 0.056 mmol).

後処理

  1. stirringthe reaction was stirred overnight at 90° C
  2. washwashed with water
  3. dry with materialdried (over anhydrous MgSO4)
  4. concentrationconcentrated in vacuo
  5. customthe residue purified by flash chromatography

出典と根拠

ORDレコード
ord-d83fd8e2ff7042a5bde14bae39fd643b
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08080571B2

反応ノート

読み込み中…

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