Triethylamine → HCID 54342534、化合物

HRID 1076189ノート

反応式

HRID 1076189 の反応式
[NH:1]=[C:2]1[N:6]=[C:5]([N:7]([CH3:9])[CH3:8])[S:4][S:3]1.[C:10]([N:14]=[C:15]=[O:16])([CH3:13])([CH3:12])[CH3:11].C(N(CC)CC)C>O1CCCC1>[C:10]([NH:14][C:15]([N:1]=[C:2]1[N:6]=[C:5]([N:7]([CH3:9])[CH3:8])[S:4][S:3]1)=[O:16])([CH3:13])([CH3:12])[CH3:11]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 62412tert-Butyl isocyanateHCID 215392483-imino-5-dimethylamino-3H-1,2,4-dithiazole

生成物 1

HCID 54342534HCID 54342534、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A suspension of 4.75 parts of the hydrobromide salt of 3-imino-5-dimethylamino-3H-1,2,4-dithiazole, two parts of t-butyl isocyanate, two parts of triethylamine, and 50 parts of tetrahydrofuran was stirred and refluxed for two days. The reaction mixture was cooled and the insoluble triethylammonium bromide was removed by filtration and discarded. The filtrate was then evaporated under reduced pressure leaving a white solid, which was recrystallized from isopropanol to afford 3.4 parts of 1-t-butyl-3-(5-dimethylamino-3H-1,2,4-dithiazol-3-ylidene)urea, m.p. 174°-177°C. dec.

後処理

  1. temperaturerefluxed for two days
  2. temperatureThe reaction mixture was cooled
  3. customthe insoluble triethylammonium bromide was removed by filtration
  4. customThe filtrate was then evaporated under reduced pressure
  5. customleaving a white solid, which
  6. customwas recrystallized from isopropanol

出典と根拠

ORDレコード
ord-28ba2993189e456fb673467b2f17fa9c
出典データセット
uspto-grants-1976_05
特許番号
US03956303

反応ノート

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