Dimethylformamide → HCID 18506854, 화합물

HRID 1355519노트

반응식

HRID 1355519 반응식
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

참가 물질

7

반응물 4

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

생성물 1

HCID 18506854HCID 18506854, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-3ce91390c9fc49b7bb54663a1c097150
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06586424B2

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