HCID 13577659、化合物 → HCID 13577665、化合物

HRID 1589214ノート

反応式

HRID 1589214 の反応式
[NH2:1][C:2]1[C:7]([CH:8]([OH:15])[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[CH:6][C:5]([Cl:16])=[CH:4][C:3]=1[CH2:17][CH2:18][OH:19]>C1C=CC=CC=1.[O-2].[O-2].[Mn+4]>[NH2:1][C:2]1[C:3]([CH2:17][CH2:18][OH:19])=[CH:4][C:5]([Cl:16])=[CH:6][C:7]=1[C:8]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=[O:15]

参加物

4

反応物 1

HCID 13577659HCID 13577659、化合物

生成物 1

HCID 13577665HCID 13577665、化合物収率 78.3%

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒HCID 241Benzene溶媒

実験手順

A suspension of 14 g (0.05 mole) of 2-amino-5-chloro-3-[hydroxy(phenyl)methyl]benzene ethanol in 500 ml of benzene was treated with 23 g (0.25 mole) of activated manganese dioxide and brought to reflux in a vessel fitted with a Dean-Stark trap. After 5 hours the hot mixture was filtered through Celite and the benzene stripped to yield a yellow material. This material was recrystallized from ethanol:pet. ether (30:60) to give 10.8 g of the titled compound, m.p. 135°-137° C.

後処理

  1. temperatureto reflux in a vessel
  2. customfitted with a Dean-Stark trap
  3. filtrationAfter 5 hours the hot mixture was filtered through Celite
  4. customto yield a yellow material
  5. customThis material was recrystallized from ethanol:pet. ether (30:60)

出典と根拠

ORDレコード
ord-8c723978ff1f4d5690cb01629776abb8
出典データセット
uspto-grants-1986_02
特許番号
US04568695

反応ノート

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