Water → HCID 70154017、化合物

HRID 1250100ノート

反応式

HRID 1250100 の反応式
[CH3:1][O:2][C:3](=[O:14])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([CH2:12][OH:13])[CH:7]=1.[C:15]1([N:21]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[C:22](Cl)=[O:23])[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.O>N1C=CC=CC=1>[CH3:1][O:2][C:3](=[O:14])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([CH2:12][O:13][C:22](=[O:23])[N:21]([C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:7]=1

参加物

5

反応物 3

HCID 962WaterHCID 65741N,N-Diphenylcarbamic chlorideHCID 21554300Acetic acid, 2-[3-(hydroxymethyl)phenoxy]-, methyl ester

生成物 1

HCID 70154017HCID 70154017、化合物収率 73.5%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

(3-Hydroxymethylphenoxy)acetic acid methyl ester (400 mg, 2 mmol) and diphenylcarbamyl chloride (580 mg, 2.5 mmol) were combined in pyridine (2 ml). The resultant yellow solution was allowed to stand for ten days under nitrogen. The mixture was then poured into water, extracted with dichloromethane, and evaporated. Purification of the residue by silica gel chromatography, eluting with 5% acetone/dichloromethane, gave {3-[(diphenyl-carbamoyloxy)methyl]phenoxy}acetic acid methyl ester as a colorless solid (575 mg, 73%).

後処理

  1. waitto stand for ten days under nitrogen
  2. extractionextracted with dichloromethane
  3. customevaporated
  4. customPurification of the residue by silica gel chromatography
  5. washeluting with 5% acetone/dichloromethane

出典と根拠

ORDレコード
ord-a032ae42ede2422c87a0821e26570e01
出典データセット
uspto-grants-2002_01
特許番号
US06335459B1

反応ノート

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