Sodium hydride → HCID 25061494、化合物

HRID 2244086ノート

反応式

HRID 2244086 の反応式
[CH3:1][C:2]1[C:10]2[C:9](=[O:11])[CH2:8][C:7]([CH3:13])([CH3:12])[CH2:6][C:5]=2[NH:4][CH:3]=1.[H-].[Na+].[CH:16]1([NH:19][C:20]2[C:29]3[C:24](=[CH:25][C:26](F)=[CH:27][CH:28]=3)[N:23]=[CH:22][N:21]=2)[CH2:18][CH2:17]1>CN(C)C=O>[CH:16]1([NH:19][C:20]2[C:29]3[C:24](=[CH:25][C:26]([N:4]4[C:5]5[CH2:6][C:7]([CH3:13])([CH3:12])[CH2:8][C:9](=[O:11])[C:10]=5[C:2]([CH3:1])=[CH:3]4)=[CH:27][CH:28]=3)[N:23]=[CH:22][N:21]=2)[CH2:18][CH2:17]1

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 248207983,6,6-trimethyl-6,7-dihydro-1H-indol-4(5H)-oneHCID 25059697N-cyclopropyl-7-fluoroquinazolin-4-amine

生成物 1

HCID 25061494HCID 25061494、化合物収率 55.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

3,6,6-Trimethyl-1,5,6,7-tetrahydro-indol-4-one (0.177 g, 1 mmol), sodium hydride (60% in oil, 40 mg, 1 mmol), Cyclopropyl-(7-fluoro-quinazolin-4-yl)-amine (0.20 g, 1 mmol), and N,N-dimethylformamide are sealed in a microwave vessel and irradiated at 100 degrees Celsius for 1500 seconds. The mixture is extracted with ethyl acetate and washed with water. The organic phase is dried over magnesium sulfate, filtered concentrated, and chromatographed to afford 0.2 g of 1-(4-Cyclopropylamino-quinazolin-7-yl)-3,6,6-trimethyl-1,5,6,7-tetrahydro-indol-4-one as a solid (55%). LC/MS m/z=361 [M+H]+.

後処理

  1. customirradiated at 100 degrees Celsius for 1500 seconds
  2. extractionThe mixture is extracted with ethyl acetate
  3. washwashed with water
  4. dry with materialThe organic phase is dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customchromatographed

出典と根拠

ORDレコード
ord-ec3e82ddc03e4fa5a6b27fe62acd4993
出典データセット
uspto-grants-2010_03
特許番号
US07678803B2

反応ノート

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