Ammonium Chloride → HCID 21322801、化合物

HRID 26342

反応式

HRID 26342 の反応式
[Cl-].[NH4+].[Cl:3][C:4]1[CH:16]=[C:15]([N+:17]([O-])=O)[CH:14]=[CH:13][C:5]=1[NH:6][CH2:7][CH:8]1[O:12][CH2:11][CH2:10][CH2:9]1>[Zn]>[ClH:3].[Cl:3][C:4]1[CH:16]=[C:15]([NH2:17])[CH:14]=[CH:13][C:5]=1[NH:6][CH2:7][CH:8]1[O:12][CH2:11][CH2:10][CH2:9]1

参加物

4

反応物 2

HCID 25517Ammonium ChlorideHCID 213228042-chloro-4-nitro-N-tetrahydrofurfurylaniline

生成物 1

HCID 21322801HCID 21322801、化合物

試薬・触媒・溶媒 1

HCID 23994Zinc触媒

実験手順

3.0 g of ammonium chloride and 50 g of zinc powder are added to 150 ml of an aqueous-alcoholic solution (85% of alcohol and 15% of water). This mixture is heated to the reflux temperature, whilst stirring, and 0.1 mol (25.7 g) of 2-chloro-4-nitro-N-tetrahydrofurfurylaniline is then added gradually. When the addition has ended and the reaction mixture is decolorised, the latter is filtered and the filtrate is collected in 20 ml of ice-cooled hydrochloric acid. After cooling, the expected hydrochloride precipitates in the form of crystals. It is filtered off, washed with a small amount of ice-cooled absolute alcohol and dried in vacuo. It melts at about 170° C. with decomposition.

後処理

  1. temperatureThis mixture is heated to the reflux temperature
  2. additionWhen the addition
  3. filtrationthe latter is filtered
  4. customthe filtrate is collected in 20 ml of ice-
  5. temperaturecooled hydrochloric acid
  6. temperatureAfter cooling
  7. customthe expected hydrochloride precipitates in the form of crystals
  8. filtrationIt is filtered off
  9. washwashed with a small amount of ice-
  10. temperaturecooled absolute alcohol
  11. customdried in vacuo

出典と根拠

ORDレコード
ord-7b37cd148ced4afebf90ae56e028634c
出典データセット
uspto-grants-1979_04
特許番号
US04149848

関連ノート

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