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Benzoyl isocyanate → 1-Benzoyl-3-(4,5,6,7-tetrahydrobenzo-[b]thien-4-yl)urea

HRID 1155644
ノート
印刷プレビュー

反応式

HRID 1155644 の反応式
[C:1]([N:9]=[C:10]=[O:11])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[S:12]1[CH:16]=[CH:15][C:14]2[CH:17]([NH2:21])[CH2:18][CH2:19][CH2:20][C:13]1=2>C(Cl)Cl>[C:1]([NH:9][C:10]([NH:21][CH:17]1[C:14]2[CH:15]=[CH:16][S:12][C:13]=2[CH2:20][CH2:19][CH2:18]1)=[O:11])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 78210Benzoyl isocyanateHCID 42163724,5,6,7-Tetrahydro-1-benzothiophen-4-amine

生成物 1

HCID 130370061-Benzoyl-3-(4,5,6,7-tetrahydrobenzo-[b]thien-4-yl)urea

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A 2.94 g sample of benzoyl isocyanate in 5 ml of CH2Cl2 is added to 3.04 g of 4,5,6,7-tetrahydrobenzo[b]thiophen-4-amine in 50 ml of CH2Cl2 under N2 atmosphere. After stirring overnight at room temperature, the reaction mixture is evaporated to dryness in vacuo. The residue is then stirred in 100 ml of Et2O and filtered to afford 1-benzoyl-3-(4,5,6,7-tetrahydrobenzo[b]thien-4-yl)urea, m.p. 189° C. to 194° C. Substitution of trichloroacetyl isocyanate for benzoyl isocyanate affords 1-trichloroacetyl-3-(4,5,6,7-tetrahydrobenzo[b]thien-4-yl)urea. Use of 4,5,6,7-tetrahydrobenzo[b]thien-4-ylisocyanate and acetamide in the above manner affords 1-acetyl-3-(4,5,6,7-tetrahydrobenzo[b]thien-4-yl)urea.

後処理

  1. customthe reaction mixture is evaporated to dryness in vacuo
  2. stirringThe residue is then stirred in 100 ml of Et2O
  3. filtrationfiltered

出典と根拠

ORDレコード
ord-469e131d73d54d6d90025cb5fad53904
出典データセット
uspto-grants-1982_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04332724

反応ノート

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