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Ethanol → 2-[-5,6-Dimethoxy-2-1H-benzimidazolylthio]-4-methoxy benzenamine

HRID 1199461
ノート
印刷プレビュー

反応式

HRID 1199461 の反応式
[CH3:1][O:2][C:3]1[C:23]([O:24][CH3:25])=[CH:22][C:6]2[NH:7][C:8]([S:10][C:11]3[CH:16]=[C:15]([O:17][CH3:18])[CH:14]=[CH:13][C:12]=3[N+:19]([O-])=O)=[N:9][C:5]=2[CH:4]=1.[Cl-].[NH4+].C(O)C.O>[Fe].CCOCC>[CH3:1][O:2][C:3]1[C:23]([O:24][CH3:25])=[CH:22][C:6]2[NH:7][C:8]([S:10][C:11]3[CH:16]=[C:15]([O:17][CH3:18])[CH:14]=[CH:13][C:12]=3[NH2:19])=[N:9][C:5]=2[CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 702EthanolHCID 962WaterHCID 25517Ammonium ChlorideHCID 198667335,6-Dimethoxy-2-(5-methoxy-2-nitrophenylthio)-1H-benzimidazole

生成物 1

HCID 198667012-[-5,6-Dimethoxy-2-1H-benzimidazolylthio]-4-methoxy benzenamine

試薬・触媒・溶媒 2

HCID 23925Iron触媒
HCID 3283
Diethyl Ether
溶媒

実験手順

The product of step (a) above (6.3 g), iron powder (6.3 g) and ammonium chloride (6.3 g) were stirred together with ethanol (63 ml) and water (120 ml) and heated under reflux for 1 hour. The hot mixture was filtered and the residue washed with hot ethyl acetate (500 ml). The combined filtrates were separated and the aqueous phase extracted with ethyl acetate. The combined ethyl acetate extracts were washed with water and brine, then dried and evaporated to leave a foam. Upon trituration with ether the sub-title compound was formed as a grey solid, MS MW bp 331.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 1 hour
  3. filtrationThe hot mixture was filtered
  4. washthe residue washed with hot ethyl acetate (500 ml)
  5. customThe combined filtrates were separated
  6. extractionthe aqueous phase extracted with ethyl acetate
  7. washThe combined ethyl acetate extracts were washed with water and brine
  8. customdried
  9. customevaporated
  10. customto leave a foam

出典と根拠

ORDレコード
ord-0b4a3e604c3a49be8057c4f868650ba0
出典データセット
uspto-grants-1990_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04900751

反応ノート

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