HCID 176526843, 화합물 → HCID 178508737, 화합물

HRID 1730783노트

반응식

HRID 1730783 반응식
Cl.[NH:2]=[C:3]1[NH:7][C:6](=[NH:8])[CH2:5][S:4]1.[NH:9]=[C:10]1[C:18]2[CH2:17][CH2:16][CH2:15][CH2:14][C:13]=2[C:12](=N)[NH:11]1>CO>[NH:9]=[C:10]1[C:18]2[CH2:17][CH2:16][CH2:15][CH2:14][C:13]=2[C:12](=[C:5]2[S:4][C:3](=[NH:2])[NH:7][C:6]2=[NH:8])[NH:11]1

참가 물질

4

반응물 2

HCID 176526843HCID 176526843, 화합물HCID 178479111HCID 178479111, 화합물

생성물 1

HCID 178508737HCID 178508737, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 6 parts of 2,4-diiminothiazolidine hydrochloride, 6 parts of 4,5,6,7-tetrahydro-1,3-diiminoisoindoline and 100 parts of anhydrous methyl alcohol was stirred and heated at reflux under an atmosphere of nitrogen for approximately 16 hours. The reaction was then cooled and filtered. The solid product collected by filtration was converted to the free base by treatment with a slight excess of a methyl alcohol solution of triethylamine and the product thus obtained was recrystallized from acetic acid. The resultant acetate salt was treated with dilute ammonium hydroxide and the product isolated to obtain in the free-base form 1-imino-4,5,6,7-tetrahydro-3(2,4-diimino-5-thiazolidinylidene)isoindoline as a greenish-brown powder melting at 215°-223° C (dec).

후처리

  1. temperatureheated
  2. temperatureat reflux under an atmosphere of nitrogen for approximately 16 hours
  3. temperatureThe reaction was then cooled
  4. filtrationfiltered
  5. filtrationThe solid product collected by filtration
  6. customthe product thus obtained
  7. customwas recrystallized from acetic acid
  8. additionThe resultant acetate salt was treated with dilute ammonium hydroxide
  9. customthe product isolated

출처 및 근거

ORD 기록
ord-29d23c5e0d704e538b839b0718314d23
출처 데이터셋
uspto-grants-1976_11
특허 번호
US03993658

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