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4-Aminoacetanilide → HCID 24877275、化合物

HRID 333406
ノート
印刷プレビュー

反応式

HRID 333406 の反応式
Br[C:2]1[CH:10]=[C:9]2[C:5](/[C:6](=[C:12]3\[O:13][C:14]([CH3:24])([CH3:23])[C:15]([N:17]4[CH2:22][CH2:21][O:20][CH2:19][CH2:18]4)=[CH:16]\3)/[C:7](=[O:11])[NH:8]2)=[CH:4][CH:3]=1.N[C:26]1[CH:31]=[CH:30][C:29]([NH:32][C:33](=[O:35])[CH3:34])=[CH:28][CH:27]=1.C1(P(C2C=CC=CC=2C2C=CC=CC=2[N:61](C)C)C2CCCCC2)CCCCC1.[Li+].C[Si]([N-][Si](C)(C)C)(C)C>C1COCC1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[CH3:23][C:14]1([CH3:24])[O:13]/[C:12](=[C:6]2/[C:7](=[O:11])[NH:8][C:9]3[C:5]/2=[CH:4][CH:3]=[C:2]([NH:61][C:27]2[CH:28]=[C:29]([NH:32][C:33](=[O:35])[CH3:34])[CH:30]=[CH:31][CH:26]=2)[CH:10]=3)/[CH:16]=[C:15]1[N:17]1[CH2:22][CH2:21][O:20][CH2:19][CH2:18]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 4

HCID 312304-AminoacetanilideHCID 2733832Lithium hexamethyldisilazaneHCID 27342172-(Dicyclohexylphosphino)-2'-(dimethylamino)biphenylHCID 24964164HCID 24964164、化合物

生成物 1

HCID 24877275HCID 24877275、化合物

試薬・触媒・溶媒 2

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
62 °C

実験手順

A 25 mL reaction flask was charged with (3E)-6-bromo-3-(5,5-dimethyl-4-morpholin-4-ylfuran-2(5H)-ylidene)-1,3-dihydro-2H-indol-2-one (100 mg, 0.26 mmol), N-(4-aminophenyl)acetamide (46 mg, 0.31 mmol), dicyclohexylphosphino-2′-(N,N-dimethylamino)biphenyl (4.9 mg, 0.012 mmol), Pd2(dba)3 (4.8 mg, 0.0052 mmol), 1M LiHMDS in THF (0.83 mL, 0.83 mmol) and dry THF (10 mL). The mixture was purged with nitrogen and heated in 62° C. bath under nitrogen for 2 hours. After cooling to room temperature, the reaction mixture was quenched with 0.5 mL of 2M HCl, and diluted with ethyl acetate (100 mL). The solution was washed with saturated NaHCO3 (2×50 mL), brine (50 mL), and concentrated to give the crude product. Purification of the crude product by silica gel chromatography with a gradient of methanol in chloroform (5-10%) led to N-(3-{[(3E)-3-(5,5-dimethyl-4-morpholin-4-ylfuran-2(5H)-ylidene)-2-oxo-2,3-dihydro-1H-indol-6-yl]amino}phenyl)acetamide as a yellow solid. Yield: 20 mg, 17%.

後処理

  1. customA 25 mL reaction flask
  2. customThe mixture was purged with nitrogen
  3. temperatureAfter cooling to room temperature
  4. customthe reaction mixture was quenched with 0.5 mL of 2M HCl
  5. additiondiluted with ethyl acetate (100 mL)
  6. washThe solution was washed with saturated NaHCO3 (2×50 mL), brine (50 mL)
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-1dbdb6ce0e2646e0b8cb0c2b682c740a
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08877923B2

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