1,2,5-Thiadiazole-3-carboxylic acid → HCID 178429215, 화합물

HRID 1762984

반응식

HRID 1762984 반응식
[S:1]1[N:5]=[CH:4][C:3]([C:6](O)=O)=[N:2]1.[NH2:9][C:10]1[CH:11]=[C:12]2[C:16](=[CH:17][C:18]=1[NH2:19])[NH:15][C:14](=[O:20])[C:13]2([CH3:22])[CH3:21]>>[CH3:21][C:13]1([CH3:22])[C:12]2[C:16](=[CH:17][C:18]3[NH:19][C:6]([C:3]4[CH:4]=[N:5][S:1][N:2]=4)=[N:9][C:10]=3[CH:11]=2)[NH:15][C:14]1=[O:20]

참가 물질

3

실험 절차

2.0 g. (15.3 mmol) 1,2,5-thiadiazole-3-carboxylic acid and 2.6 g. (13.6 mmol) 5,6-diamino-3,3-dimethyl-indolin-2-one are heated in 40 ml. polyphosphoric acid under an atmosphere of nitrogen for 2 hours at 160° C. The warm solution is poured on to ice water, worked up and the crystals obtained are filtered off with suction. The residue is again suspended in water, neutralised with an aqueous solution of ammonia, filtered off with suction and recrystallised from methanol with the addition of charcoal. Yield: 2.6 g. (66% of theory); m.p. >300° C.

후처리

  1. customthe crystals obtained
  2. filtrationare filtered off with suction
  3. filtrationfiltered off with suction
  4. customrecrystallised from methanol with the addition of charcoal

출처 및 근거

ORD 기록
ord-b7abef2b545641bb89caf351f6761fe4
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04835280

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