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2-Isocyanatoethyl propionate → HCID 13053835、化合物

HRID 1702870
ノート
印刷プレビュー

反応式

HRID 1702870 の反応式
[OH:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][C:8](=[O:10])[S:7][C:6]=2[CH:11]=1.[C:12]([O:16][CH2:17][CH2:18][N:19]=[C:20]=[O:21])(=[O:15])[CH2:13][CH3:14]>C([O-])(=O)CCCCCCCCCCC.C([O-])(=O)CCCCCCCCCCC.C([Sn+2]CCCC)CCC.C(C(C)=O)C>[C:12]([O:16][CH2:17][CH2:18][NH:19][C:20]([O:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][C:8](=[O:10])[S:7][C:6]=2[CH:11]=1)=[O:21])(=[O:15])[CH2:13][CH3:14]
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 1343472-Isocyanatoethyl propionateHCID 1390671,3-Benzoxathiol-2-one, 5-hydroxy-

生成物 1

HCID 13053835HCID 13053835、化合物

試薬・触媒・溶媒 2

HCID 9809426Di-n-butyldilauryltin触媒HCID 6569Methyl Ethyl Ketone溶媒

実験手順

5-hydroxy-1,3-benzoxathiol-2-one (16.8 grams) was mixed with 2-(isocyanato)ethyl propionate (15.0 grams) and 10 drops of dibutyltin dilaurate in 200 milliliters of methyl ethyl ketone. The resulting solution was heated at reflux temperature for four hours and fifteen minutes, after which the solvent was removed by evaporation in vacuo, leaving a brown, viscous oil which crystallized upon standing at room temperature for 10 to 15 hours. The crude product was twice recrystallized from toluene. The purified compound, 5-[2-(propionyloxy)ethylcarbamoyloxy]-1,3-benzoxathiol-2-one, was a white, fibrous crystalline substance with a melting point of 78°-79° C. Elemental analysis calculated for C13H13NO6S (percent): carbon--50.15; hydrogen--4.21; nitrogen--4.50. Found: carbon--50.4; hydrogen--4.27; nitrogen--4.45.

後処理

  1. temperatureThe resulting solution was heated
  2. temperatureat reflux temperature for four hours
  3. customfifteen minutes, after which the solvent was removed by evaporation in vacuo
  4. customleaving a brown, viscous oil which
  5. customcrystallized
  6. customThe crude product was twice recrystallized from toluene

出典と根拠

ORDレコード
ord-4d087224fe8f46fd89ab2ff34a13d087
出典データセット
uspto-grants-1982_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04349685

反応ノート

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