Methyl chloroacetate → HCID 59253951、化合物

HRID 83811

反応式

HRID 83811 の反応式
[N+:1]([C:4]1[CH:14]=[CH:13][C:7]([O:8][CH2:9][C:10]([OH:12])=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2].C(N(CC)CC)C.Cl[CH2:23][C:24]([O:26][CH3:27])=[O:25]>CC(C)=O>[CH3:27][O:26][C:24]([CH2:23][O:11][C:10](=[O:12])[CH2:9][O:8][C:7]1[CH:6]=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:14][CH:13]=1)=[O:25]

参加物

5

反応物 3

HCID 7295Methyl chloroacetateHCID 8471TriethylamineHCID 15720(4-Nitrophenoxy)acetic acid

生成物 1

HCID 59253951HCID 59253951、化合物収率 90.8%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a mixture of (4-nitrophenoxy)acetic acid 22 (150 g, 761.4 mmol) and triethyl-amine (85 g, 840 mmol) in acetone (750 ml) was added methyl chloroacetate (91.6 g, 844 mmol) drop wise and stirred under reflux for 8 hours. Solids were filtered off and poured onto cold 5% sodium bicarbonate solution (4 L). Crude 44 was filtered, dried and recrystallised from chloroform:hexane (1:6) to get pure 44 (186 g, 90.8%) as a white powder with an m.p. between 88-90° C.

後処理

  1. temperatureunder reflux for 8 hours
  2. filtrationSolids were filtered off
  3. additionpoured onto cold 5% sodium bicarbonate solution (4 L)
  4. filtrationCrude 44 was filtered
  5. customdried
  6. customrecrystallised from chloroform:hexane (1:6)

出典と根拠

ORDレコード
ord-d17d530434914752a853376796162732
出典データセット
uspto-grants-2014_09
特許番号
US08846845B2

関連ノート

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