Dimethylformamide → HCID 18506854、化合物

HRID 1355519ノート

反応式

HRID 1355519 の反応式
O[CH2:2][C:3]1[N:8]=[C:7]([NH:9][C:10]2[S:11][C:12]([C:15]#[N:16])=[CH:13][N:14]=2)[CH:6]=[CH:5][CH:4]=1.CN(C=O)C.O=P(Cl)(Cl)[Cl:24].C([O-])(O)=O.[Na+]>C(Cl)Cl.O>[Cl:24][CH2:2][C:3]1[N:8]=[C:7]([NH:9][C:10]2[S:11][C:12]([C:15]#[N:16])=[CH:13][N:14]=2)[CH:6]=[CH:5][CH:4]=1

参加物

7

反応物 4

HCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 516892Sodium BicarbonateHCID 185069372-(6-Hydroxymethyl-pyridin-2-ylamino)-thiazole-5-carbonitrile

生成物 1

HCID 18506854HCID 18506854、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

2-(6-Hydroxymethyl-pyridin-2-ylamino)-thiazole-5-carbonitrile (0.300 g, 0.29 mmol) was stirred in 5 mL anh DCM under N2. Anhydrous DMF (0.100 mL, 1.29 mmol) and POCl3 (0.120 mL, 1.29 mmol) were added. After 15 h the reaction was diluted with water and the pH was adjusted to 9 with sat NaHCO3 (aq). The dCM was removed in vacuo and the precipitate which formed was filtered and washed with water to provide the titled compound. 1H NMR (DMSO-d6) δ 12.35 (s, 1H), 8.29 (s, 1H), 7.85 (t, 1H, J=7.8 Hz), 7.21 (d, 1H, 7.3 Hz), 7.11 (d, 1H, 8.2 Hz), 4.85 (s, 2H).

後処理

  1. customThe dCM was removed in vacuo
  2. customthe precipitate which formed
  3. filtrationwas filtered
  4. washwashed with water

出典と根拠

ORDレコード
ord-3ce91390c9fc49b7bb54663a1c097150
出典データセット
uspto-grants-2003_07
特許番号
US06586424B2

反応ノート

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