[4-(4-Nitrophenoxy)phenyl]acetic acid → HCID 20392568、化合物

HRID 1704011ノート

反応式

HRID 1704011 の反応式
[N+:1]([C:4]1[CH:20]=[CH:19][C:7]([O:8][C:9]2[CH:14]=[CH:13][C:12]([CH2:15][C:16]([OH:18])=[O:17])=[CH:11][CH:10]=2)=[CH:6][CH:5]=1)([O-])=O>C(O)C.[Pt]=O>[NH2:1][C:4]1[CH:5]=[CH:6][C:7]([O:8][C:9]2[CH:14]=[CH:13][C:12]([CH2:15][C:16]([OH:18])=[O:17])=[CH:11][CH:10]=2)=[CH:19][CH:20]=1

参加物

4

反応物 1

HCID 10858649[4-(4-Nitrophenoxy)phenyl]acetic acid

生成物 1

HCID 20392568HCID 20392568、化合物収率 40.3%

試薬・触媒・溶媒 2

HCID 82844Platinum oxide (PtO)触媒HCID 702Ethanol溶媒

実験手順

To a solution of 13.65 g of [p-(p-nitrophenoxy)-phenyl]acetic acid in 100 ml of ethanol is added 130 mg of platinum oxide. The mixture is shaken under 45 lb hydrogen pressure in a Parr shaker. After 2 hours, a thick white solid precipitates. The mixture is filtered, and 200 mg of fresh platinum oxide is added to the filtrate which is subjected to the reducing conditions. After an additional hour, the mixture is filtered and washed with cold ethanol. The combined solids are dissolved in hot methanol and filtered. Water is added to the filtrate to afford 4.9 g of a brown solid. A portion is recrystallized from methanol to yield the product as cream colored crystals, mp 172° C (dec.).

後処理

  1. customa thick white solid precipitates
  2. filtrationThe mixture is filtered
  3. addition200 mg of fresh platinum oxide is added to the filtrate which
  4. waitAfter an additional hour
  5. filtrationthe mixture is filtered
  6. washwashed with cold ethanol
  7. dissolutionThe combined solids are dissolved in hot methanol
  8. filtrationfiltered
  9. additionWater is added to the filtrate

出典と根拠

ORDレコード
ord-3720b5b5fc68400e99e6c76739f9998d
出典データセット
uspto-grants-1978_11
特許番号
US04125729

反応ノート

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