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Dimethylformamide → 3-[4'-(2,3-dihydroindole-1-carbonyl)-3,4,5,6-tetrahydro-2H-1,2'-bipyridinyl-4-yl]-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one

HRID 74620
ノート
印刷プレビュー

反応式

HRID 74620 の反応式
[NH:1]1[CH2:6][CH2:5][CH:4]([N:7]2[CH2:13][CH2:12][C:11]3[CH:14]=[CH:15][CH:16]=[CH:17][C:10]=3[NH:9][C:8]2=[O:18])[CH2:3][CH2:2]1.Cl[C:20]1[CH:25]=[C:24]([C:26]([N:28]2[C:36]3[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=3)[CH2:30][CH2:29]2)=[O:27])[CH:23]=[CH:22][N:21]=1.CCN(C(C)C)C(C)C.CN(C=O)C>O>[N:28]1([C:26]([C:24]2[CH:23]=[CH:22][N:21]=[C:20]([N:1]3[CH2:2][CH2:3][CH:4]([N:7]4[CH2:13][CH2:12][C:11]5[CH:14]=[CH:15][CH:16]=[CH:17][C:10]=5[NH:9][C:8]4=[O:18])[CH2:5][CH2:6]3)[CH:25]=2)=[O:27])[C:36]2[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=2)[CH2:30][CH2:29]1
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 4

HCID 6228DimethylformamideHCID 81531DiisopropylethylamineHCID 113795873-(Piperidin-4-yl)-4,5-dihydro-1H-benzo[d][1,3]diazepin-2(3H)-oneHCID 28376039(2-Chloropyridin-4-yl)-(2,3-dihydroindol-1-yl)-methanone

生成物 1

HCID 426131403-[4'-(2,3-dihydroindole-1-carbonyl)-3,4,5,6-tetrahydro-2H-1,2'-bipyridinyl-4-yl]-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one

試薬・触媒・溶媒

1
HCID 962Water溶媒

実験手順

100 mg (0.41 mmol) 3-piperidin-4-yl-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one were added to 110 mg (0.43 mmol) (2-chloropyridin-4-yl)-(2,3-dihydro-indol-1-yl)-methanone and 3.0 mL (17.4 mmol) DIPEA. The reaction mixture was refluxed for 5 h with stirring. Then 1 mL DMF were added and the mixture was stirred overnight at 130 C. After cooling water was added, the precipitate formed was suction filtered and purified by preparative HPLC. The product fractions were combined and evaporated down i. vac.

後処理

  1. temperatureThe reaction mixture was refluxed for 5 h
  2. stirringthe mixture was stirred overnight at 130 C
  3. additionwas added
  4. customthe precipitate formed
  5. filtrationfiltered
  6. custompurified by preparative HPLC
  7. customevaporated down i

出典と根拠

ORDレコード
ord-a67b466eac1746d88a2475bc793126c1
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08829006B2

反応ノート

読み込み中…

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