Morpholine → 7-morpholin-4-yl-3H-benzo[d]-1,2,3-triazin-4-one

HRID 714762ノート

反応式

HRID 714762 の反応式
F[C:2]1[CH:3]=[CH:4][C:5]2[C:10](=[O:11])[NH:9][N:8]=[N:7][C:6]=2[CH:12]=1.[NH:13]1[CH2:18][CH2:17][O:16][CH2:15][CH2:14]1>>[N:13]1([C:2]2[CH:3]=[CH:4][C:5]3[C:10](=[O:11])[NH:9][N:8]=[N:7][C:6]=3[CH:12]=2)[CH2:18][CH2:17][O:16][CH2:15][CH2:14]1

参加物

3

反応物 2

HCID 8083MorpholineHCID 1361028587-Fluoro-3,4-dihydro-1,2,3-benzotriazin-4-one

生成物 1

HCID 1362722027-morpholin-4-yl-3H-benzo[d]-1,2,3-triazin-4-one

実験手順

32.5 g (0.196 mol) of 7-fluoro-3H-benzo[d]-1,2,3-triazin-4-one were heated at 120° C. for 5 hours in 300 ml of morpholine with stirring. The precipitated product was filtered off with suction at 50° C., the precipitate was washed with water, filtered off with suction and dried in a vacuum drying cabinet for 48 hours, giving 30.5 g of 7-morpholin-4-yl-3H-benzo[d]-1,2,3-triazin-4-one as solid; 1H NMR (500 MHz, DMSO) δ 8.00 (d, J=9.0, 1H), 7.52 (dd, J=9.0, 2.6, 1H), 7.39 (dd, J=22.8, 2.6, 1H), 3.78 (dd, J=17.1, 12.3, 4H), 3.45 (dd, J=17.1, 12.3, 4H).

後処理

  1. filtrationThe precipitated product was filtered off with suction at 50° C.
  2. washthe precipitate was washed with water
  3. filtrationfiltered off with suction
  4. customdried in a vacuum
  5. customdrying cabinet for 48 hours

出典と根拠

ORDレコード
ord-cd085885608c475e88569e5bd3f28cf8
出典データセット
uspto-grants-2015_11
特許番号
US09187469B2

反応ノート

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