Hydrochloric Acid → 4-Chloro-7-methyl-1,2,3-triazino[4',5'-4,5]thiopheno[2,3-b]pyridine

HRID 1732918ノート

反応式

HRID 1732918 の反応式
[NH2:1][C:2]1[C:10]2[C:5](=[N:6][C:7]([CH3:11])=[CH:8][CH:9]=2)[S:4][C:3]=1[C:12]#[N:13].[ClH:14].[N:15]([O-])=O.[Na+]>O>[Cl:14][C:12]1[C:3]2[S:4][C:5]3[N:6]=[C:7]([CH3:11])[CH:8]=[CH:9][C:10]=3[C:2]=2[N:1]=[N:15][N:13]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 7023133-Amino-6-methylthieno[2,3-b]pyridine-2-carbonitrileHCID 23668193Sodium Nitrite

生成物 1

HCID 4607114-Chloro-7-methyl-1,2,3-triazino[4',5'-4,5]thiopheno[2,3-b]pyridine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a cold solution of 4.2 g. (0.022 M) of 3-amino-2-cyano-6-methylthieno[2,3-b]pyridine in 30 ml. conc. HCl and 30 ml. HOAC was added a solution of 1.9 g. (0.028 M) of NaNO2 in 20 ml. of H2O. After completion of addition, the ice bath was removed and stirring continued for 2 more hours. The mixture was then poured on ice water and filtered. The crude product was recrystallized from methanol, m.p. 188°-189° C.

後処理

  1. additionHOAC was added a solution of 1.9 g
  2. additionAfter completion of addition
  3. customthe ice bath was removed
  4. additionThe mixture was then poured on ice water
  5. filtrationfiltered
  6. customThe crude product was recrystallized from methanol, m.p. 188°-189° C.

出典と根拠

ORDレコード
ord-c7dec922fb38482a83ffab16ba59e992
出典データセット
uspto-grants-1980_12
特許番号
US04239887

反応ノート

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