Acetic Acid → HCID 178502014、化合物

HRID 437796ノート

反応式

HRID 437796 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([C:13]3[CH:14]=[C:15]([NH2:20])[C:16]([NH2:19])=[CH:17][CH:18]=3)[O:12][CH2:11][CH2:10][O:9]2)=[CH:4][CH:3]=1.[CH3:21][O:22][C:23]([NH:25][C:26](=NC(=O)OC)SC)=[O:24].C(O)(=O)C>ClC(Cl)Cl>[CH3:21][O:22][C:23](=[O:24])[NH:25][C:26]1[NH:19][C:16]2[CH:17]=[CH:18][C:13]([C:8]3([C:5]4[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=4)[O:9][CH2:10][CH2:11][O:12]3)=[CH:14][C:15]=2[N:20]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 98708Methyl [[(methoxycarbonyl)amino](methylthio)methylene]carbamateHCID 64548874-(2-(4-Fluorophenyl)-1,3-dioxolan-2-yl)benzene-1,2-diamine

生成物 1

HCID 178502014HCID 178502014、化合物収率 42%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A mixture of 5.5 parts of 4-[2-(4-fluorophenyl)-1,3-dioxolan2-yl]-1,2-benzenediamine, 6.2 parts of methyl [(methoxycarbonylamino)(methylthio)methylene]carbamate, 4.8 parts of acetic acid and 225 parts of trichloromethane is stirred and refluxed for 17 hours. The reaction mixture is evaporated in vacuo. The residue is triturated in methanol. The product is filtered off, washed with 2,2' -oxybispropane and dried, yielding 3 parts (42%) of methyl{ 5-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]-1H-benzimidazol-2-yl}carbamate; mp. 227.7° C.

後処理

  1. temperaturerefluxed for 17 hours
  2. customThe reaction mixture is evaporated in vacuo
  3. customThe residue is triturated in methanol
  4. filtrationThe product is filtered off
  5. washwashed with 2,2' -oxybispropane
  6. customdried

出典と根拠

ORDレコード
ord-ebe53c538602438484bd819ffa199270
出典データセット
uspto-grants-1977_06
特許番号
US04032536

反応ノート

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