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

HRID 1732918노트

반응식

HRID 1732918 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-c7dec922fb38482a83ffab16ba59e992
출처 데이터셋
uspto-grants-1980_12
특허 번호
US04239887

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