HCID 57435373、化合物 → HCID 57513765、化合物

HRID 2368432ノート

反応式

HRID 2368432 の反応式
[CH2:1]([N:8]1[C:12]([C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=2)=[N:11][C:10]([NH2:20])=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:21]([O:28][C:29]1[O:30][C:31](=[O:36])[C:32]([CH3:35])([CH3:34])[N:33]=1)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>C1(C)C=CC=CC=1>[CH2:21]([O:28][C:29](=[O:30])[NH:33][C:32]([C:31](=[O:36])[NH:20][C:10]1[N:11]=[C:12]([C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=2)[N:8]([CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[N:9]=1)([CH3:34])[CH3:35])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1

参加物

4

反応物 2

HCID 57435373HCID 57435373、化合物HCID 57435374HCID 57435374、化合物

生成物 1

HCID 57513765HCID 57513765、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
50 °C

実験手順

1-Benzyl-5-(4-fluorophenyl)-1H-1,2,4-triazol-3-amine (4.15 g, 15.47 mmol), 2-(benzyloxy)-4,4-dimethyloxazol-5(4H)-one (4.07 g, 18.56 mmol) were stirred in 5 ml of toluene in a 100 ml prbf. The white suspension was allowed to stir at 50° C. for over weekend. It was then cooled to r.t. The volatiles were removed in vacuo and the resulted solid was dissolved in EtOAc (130 mL) and heptane (50 mL) with heating. It was cooled to r.t. and let sit overnight. The resulted precipitates were collected and dried to afford the title compound. 1H NMR (400 MHz, DMSO-d6) 1.41 (s, 6H) 5.01 (s, 2H) 5.43 (s, 2H) 7.12 (d, J=6.82 Hz, 2H) 7.23-7.43 (m, 11H) 7.64-7.74 (m, 2H), 10.05 (br. s., 1H). MS (m/z) 488.1 M(+1), tR=1.60, Method A.

後処理

  1. temperatureIt was then cooled to r.t
  2. customThe volatiles were removed in vacuo
  3. dissolutionthe resulted solid was dissolved in EtOAc (130 mL)
  4. temperatureheptane (50 mL) with heating
  5. temperatureIt was cooled to r.t.
  6. customThe resulted precipitates
  7. customwere collected
  8. customdried

出典と根拠

ORDレコード
ord-a2d049a160b546a8a45e00ceb765feab
出典データセット
uspto-grants-2014_04
特許番号
US08703761B2

反応ノート

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