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 1701138노트

반응식

HRID 1701138 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 3776Isopropanol용매

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온도
-15 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6ceef21f65b04064991a3d0891078ccb
출처 데이터셋
uspto-grants-1980_03
특허 번호
US04191768

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