Acetic Acid → 7-Bromo-1,2,4,5-tetrahydro-pyrido[2,3-e][1,4]diazepin-3-one

HRID 1362359ノート

反応式

HRID 1362359 の反応式
[NH:1]1[C:7]2[N:8]=[CH:9][CH:10]=[CH:11][C:6]=2[CH2:5][NH:4][C:3](=[O:12])[CH2:2]1.C(O)(=O)C.[Br:17]Br>CCCCCC>[Br:17][C:10]1[CH:9]=[N:8][C:7]2[NH:1][CH2:2][C:3](=[O:12])[NH:4][CH2:5][C:6]=2[CH:11]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 24408BromineHCID 592775691H,2H,3H,4H,5H-pyrido[2,3-e][1,4]diazepin-3-one

生成物 1

HCID 592776207-Bromo-1,2,4,5-tetrahydro-pyrido[2,3-e][1,4]diazepin-3-one

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

1,2,4,5-Tetrahydro-pyrido[2,3-e][1,4]diazepin-3-one (164 mg, 1.0 mmol) was dissolved into acetic acid (1 mL). Bromine (160 mg, 1.0 mmol) was added dropwise at room temperature and the solution was stirred overnight. Hexane (5 mL) was added and the orange precipitate was filtered and dried in vacuo. The title compound was isolated as an orange solid (190 mg, 78%). 1H NMR (300 MHz, DMSO-d6) δ 8.26 (t, J=5.7 Hz, 1H), 8.06 (d, J=2.1 Hz, 1H), 7.81 (d, J=2.1 Hz, 1H), 4.35 (d, J=5.7 Hz, 2H), 4.08 (s, 2H).

後処理

  1. filtrationthe orange precipitate was filtered
  2. customdried in vacuo

出典と根拠

ORDレコード
ord-54529094ddf447a5a00e47eeea3b1bb0
出典データセット
uspto-grants-2011_02
特許番号
US07879872B2

反応ノート

読み込み中…