Triphosgene → HCID 89445050、化合物

HRID 526041

反応式

HRID 526041 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([NH2:8])[C:3]=1[N:9]1[CH:13]=[CH:12][CH:11]=[CH:10]1.Cl[C:15](Cl)([O:17]C(=O)OC(Cl)(Cl)Cl)Cl>C1(C)C=CC=CC=1>[CH3:1][C:2]1[C:3]2[N:9]3[CH:13]=[CH:12][CH:11]=[C:10]3[C:15](=[O:17])[NH:8][C:4]=2[N:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 94429TriphosgeneHCID 894449024-Methyl-3-(1H-pyrrol-1-yl)pyridine-2-amine

生成物 1

HCID 89445050HCID 89445050、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

4-Methyl-3-(1H-pyrrol-1-yl)pyridine-2-amine (1.0 g, 5.8 mmol) and triphosgene (2.6 g, 8.7 mmol) were dissolved in 100 mL of toluene. The mixture was refluxed for 3 hours, then cooled to room temperature. The red solid was collected after filtration and washed with CH3CN 0.5 g (43%). The material was used directly for the next step reaction without purification. 1H NMR (400 MHz, DMSO) δ 11.64 (s, 1H), 8.15 (dd, J=1.4, 2.9 Hz, 1H), 8.13 (d, J=4.9 Hz, 1H), 7.20-7.08 (m, 2H), 6.75 (dd, J=2.9, 3.9 Hz, 1H), 2.81 (s, 3H).

後処理

  1. temperatureThe mixture was refluxed for 3 hours
  2. customThe red solid was collected
  3. filtrationafter filtration
  4. washwashed with CH3CN 0.5 g (43%)
  5. customThe material was used directly for the next step reaction without purification

出典と根拠

ORDレコード
ord-1fe23c41d3094d718234d7bffddc7c75
出典データセット
uspto-grants-2016_05
特許番号
US09345703B2

関連ノート

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