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creatinine → HCID 136074472、化合物

HRID 904172
ノート
印刷プレビュー

反応式

HRID 904172 の反応式
[CH3:1][N:2]1[C:7]([NH2:8])=[N:6][C:4](=[O:5])[CH2:3]1.[O:9]1[CH:13]=[CH:12][C:11]([N:14]=[C:15]=[O:16])=[CH:10]1>CN(C=O)C.C1(C)C=CC=CC=1>[O:9]1[CH:13]=[CH:12][C:11]([NH:14][C:15]([N:8]=[C:7]2[NH:6][C:4](=[O:5])[CH2:3][N:2]2[CH3:1])=[O:16])=[CH:10]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 588creatinineHCID 115283353-Isocyanatofuran

生成物 1

HCID 136074472HCID 136074472、化合物収率 1.4%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a stirred mixture of 18.3 g (162 mM) of creatinine in 120 ml of anhydrous DMF was added a solution of 17.2 g (162 mM) of 3-furanyl isocyanate in 80 ml of toluene. After stirring the mixture for 3 hrs. at 65° C., the mixture was partially concentrated under vacuum and the residue poured into 1200 ml of water. The resulting precipitate was collected, washed with water and recrystallized from ethyl acetate. The solid was then chromatographed over silica gel using ethyl acetate as the eluant and the fractions containing the product were concentrated and the residue recrystallized from toluene to give 0.5 g of the above urea as a tan solid, m.p. 179°-181° C. (dec.).

後処理

  1. concentrationat 65° C., the mixture was partially concentrated under vacuum
  2. additionthe residue poured into 1200 ml of water
  3. customThe resulting precipitate was collected
  4. washwashed with water
  5. customrecrystallized from ethyl acetate
  6. customThe solid was then chromatographed over silica gel
  7. additionthe fractions containing the product
  8. concentrationwere concentrated
  9. customthe residue recrystallized from toluene

出典と根拠

ORDレコード
ord-32fcc878990c42e8b5fbc377663e90f6
出典データセット
uspto-grants-1980_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04230713

反応ノート

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