1,3-Diazepan-2-one hydrazone hydroiodide → 1,5-Bis[p-(trifluoromethoxy)phenyl]-1,4-pentadien-3-one-4,5,6,7-tetrahydro-1H-1,3-diazepin-2-ylhydrazone

HRID 1701138ノート

反応式

HRID 1701138 の反応式
[F:1][C:2]([F:28])([F:27])[O:3][C:4]1[CH:9]=[CH:8][C:7]([CH:10]=[CH:11][C:12](=O)[CH:13]=[CH:14][C:15]2[CH:20]=[CH:19][C:18]([O:21][C:22]([F:25])([F:24])[F:23])=[CH:17][CH:16]=2)=[CH:6][CH:5]=1.I.[NH:30]1[CH2:36][CH2:35][CH2:34][CH2:33][N:32]=[C:31]1[NH:37][NH2:38]>C(O)(C)C>[NH:32]1[CH2:33][CH2:34][CH2:35][CH2:36][N:30]=[C:31]1[NH:37][N:38]=[C:12]([CH:13]=[CH:14][C:15]1[CH:20]=[CH:19][C:18]([O:21][C:22]([F:25])([F:24])[F:23])=[CH:17][CH:16]=1)[CH:11]=[CH:10][C:7]1[CH:8]=[CH:9][C:4]([O:3][C:2]([F:28])([F:27])[F:1])=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 131940841,3-Diazepan-2-one hydrazone hydroiodideHCID 543760901,5-Bis[p-(trifluoromethoxy)phenyl]-1,4-pentadien-3-one

生成物 1

HCID 570149011,5-Bis[p-(trifluoromethoxy)phenyl]-1,4-pentadien-3-one-4,5,6,7-tetrahydro-1H-1,3-diazepin-2-ylhydrazone収率 75%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
-15 °C

実験手順

A mixture of 1,5-bis[p-(trifluoromethoxy)phenyl]-1,4-pentadien-3-one (4.0 g; 0.01 mole), 4,5,6,7-tetrahydro-1H-1,3-diazepine-2-ylhydrazine hydroiodide (2.6 g; 0.01 mole) and isopropyl alcohol (25 ml) is heated at reflux for 2 to 3 hours. The reaction mixture is then cooled to -15° C., and the precipitated material is isolated by filtration and washed with ether. The isolated material is mixed with ether and saturated sodium carbonate solution and the mixture stirred for about 15 minutes. The ether layer is then separated, dried, and concentrated to afford 3.8 g (75%) of title product, a bright yellow solid, m.p. 184.5°-185.5° C.

後処理

  1. temperatureis heated
  2. temperatureat reflux for 2 to 3 hours
  3. customthe precipitated material is isolated by filtration
  4. washwashed with ether
  5. additionThe isolated material is mixed with ether and saturated sodium carbonate solution
  6. customThe ether layer is then separated
  7. customdried
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-6ceef21f65b04064991a3d0891078ccb
出典データセット
uspto-grants-1980_03
特許番号
US04191768

反応ノート

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