HCID 176526843、化合物 → HCID 178508737、化合物

HRID 1833501ノート

反応式

HRID 1833501 の反応式
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

参加物

4

反応物 2

HCID 176526843HCID 176526843、化合物HCID 178479111HCID 178479111、化合物

生成物 1

HCID 178508737HCID 178508737、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-77445322b1dc4077a85978a2e07b7efa
出典データセット
uspto-grants-1978_01
特許番号
US04066653

反応ノート

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