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Acetic Acid → 2-(gamma-Hydroxypropyl)amino-6-(gamma-hydroxypropyl)aminonitrobenzene

HRID 2291442
ノート
印刷プレビュー

反応式

HRID 2291442 の反応式
Cl[C:2]1[CH:7]=[C:6]([NH:8][CH2:9][CH2:10][CH2:11][OH:12])[C:5]([N+:13]([O-:15])=[O:14])=[C:4]([NH:16][CH2:17][CH2:18][CH2:19][OH:20])[CH:3]=1.C(O)(=O)C.C(O)=O.O>C(N(CC)CC)C.[Pd]>[OH:20][CH2:19][CH2:18][CH2:17][NH:16][C:4]1[CH:3]=[CH:2][CH:7]=[C:6]([NH:8][CH2:9][CH2:10][CH2:11][OH:12])[C:5]=1[N+:13]([O-:15])=[O:14]
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 176Acetic AcidHCID 284Formic AcidHCID 962WaterHCID 200710684-Chloro-2-(gamma-hydroxypropyl)amino-6-(gamma-hydroxypropyl)aminonitrobenzene

生成物 1

HCID 200710672-(gamma-Hydroxypropyl)amino-6-(gamma-hydroxypropyl)aminonitrobenzene

試薬・触媒・溶媒 2

HCID 23938Palladium
触媒
HCID 8471Triethylamine溶媒

実験手順

340 mg of palladium at a concentration of 10% on calcium carbonate are added to 0.017 mole (5.2 g) of 4- chloro-2-(γ-hydroxypropyl)amino-6-(γ-hydroxypropyl)aminonitrobenzene in 11.7 ml of triethylamine. 0.9 ml of acetic acid and 2.3 ml of formic acid are then run in dropwise. A high exothermicity is noted. The reaction mixture is heated under reflux for 3 hours. 10 ml of water are added. The reaction mixture diluted in this manner is filtered hot to remove the catalyst. The expected product precipitates from the filtrate as it cools. It is filtered off, washed with water and then dried under vacuum in the presence of phosphorus pentoxide. Recrystallized from ethyl acetate, it melts at 90° C.

後処理

  1. temperatureThe reaction mixture is heated
  2. temperatureunder reflux for 3 hours
  3. additionThe reaction mixture diluted in this manner
  4. filtrationis filtered hot
  5. customto remove the catalyst
  6. customThe expected product precipitates from the filtrate as it
  7. filtrationIt is filtered off
  8. washwashed with water
  9. dry with materialdried under vacuum in the presence of phosphorus pentoxide
  10. customRecrystallized from ethyl acetate, it melts at 90° C.

出典と根拠

ORDレコード
ord-36737dbb1b93463c8dac468f564b8e3c
出典データセット
uspto-grants-1989_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04797129

反応ノート

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