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1-[5-bromo-1-(3-methyl-butyl)-1H-benzoimidazol-2-ylmethyl]-3-isopropyl-1,3-dihydro-benzoimidazol-2-one → HCID 20813973、化合物

HRID 896333
ノート
印刷プレビュー

反応式

HRID 896333 の反応式
Br[C:2]1[CH:29]=[CH:28][C:5]2[N:6]([CH2:23][CH2:24][CH:25]([CH3:27])[CH3:26])[C:7]([CH2:9][N:10]3[C:14]4[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=4[N:12]([CH:19]([CH3:21])[CH3:20])[C:11]3=[O:22])=[N:8][C:4]=2[CH:3]=1.[CH2:30](C([Sn])=C(CCCC)CCCC)[CH2:31]CC>C1(C)C=CC=CC=1.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>[CH:19]([N:12]1[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[N:10]([CH2:9][C:7]2[N:6]([CH2:23][CH2:24][CH:25]([CH3:27])[CH3:26])[C:5]3[CH:28]=[CH:29][C:2]([CH:30]=[CH2:31])=[CH:3][C:4]=3[N:8]=2)[C:11]1=[O:22])([CH3:21])[CH3:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 208139981-[5-bromo-1-(3-methyl-butyl)-1H-benzoimidazol-2-ylmethyl]-3-isopropyl-1,3-dihydro-benzoimidazol-2-oneHCID 53438229Tri(butyl)vinyltin

生成物 1

HCID 20813973HCID 20813973、化合物収率 32.3%

試薬・触媒・溶媒 3

HCID 178418397HCID 178418397、化合物触媒HCID 1140Toluene
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 1-[5-bromo-1-(3-methyl-butyl)-1H-benzoimidazol-2-ylmethyl]-3-isopropyl-1,3-dihydro-benzoimidazol-2-one (90 mg, 0.2 mmol), tributylvinyltin (76 mg, 0.24 mmol) and tetrakis(triphenylphosphine)palladium(0) (23 mg, 0.02 mmol) in toluene (4 mL) was heated to reflux for 4 h. After cooling, the reaction mixture was diluted with EtOAc and washed with sat. NaHCO3 and brine. The organic layer was dried over MgSO4 and evaporated. The residue was purified by flash chromatography (hexanes:EtOAc 4:1 to 2:1) to give 26 mg (32%) of 1-isopropyl-3-[1-(3-methyl-butyl)-5-vinyl-1H-benzoimidazol-2-ylmethyl]-1,3-dihydro-benzoimidazol-2-one as a off-white solid.

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 4 h
  3. temperatureAfter cooling
  4. washwashed with sat. NaHCO3 and brine
  5. dry with materialThe organic layer was dried over MgSO4
  6. customevaporated
  7. customThe residue was purified by flash chromatography (hexanes:EtOAc 4:1 to 2:1)

出典と根拠

ORDレコード
ord-2bf49f8e5cff4ed08ea16878901b0ebe
出典データセット
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06919331B2

反応ノート

読み込み中…

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