Benzyl Alcohol → HCID 18370146、化合物

HRID 484752ノート

反応式

HRID 484752 の反応式
[CH3:1][CH:2]([CH3:10])[CH2:3][CH2:4][C:5](=[O:9])[C:6]([OH:8])=[O:7].C1(N=C=NC2CCCCC2)CCCCC1.[CH2:26](O)[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1>C(Cl)Cl>[CH3:1][CH:2]([CH3:10])[CH2:3][CH2:4][C:5](=[O:9])[C:6]([O:8][CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)=[O:7]

参加物

5

反応物 3

HCID 244Benzyl AlcoholHCID 10868DicyclohexylcarbodiimideHCID 1293965126395-06-2

生成物 1

HCID 18370146HCID 18370146、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
-15 °C

実験手順

A solution of 5-methyl-2-oxohexanoic acid (0.288 g.) in methylene chloride (1 ml.) was added during 15 minutes to a stirred solution of dicyclohexylcarbodiimide (0.412 g.) and benzyl alcohol (0.432 g.) in methylene chloride (10 ml.) which was cooled to -15° C., and the mixture was stirred at that temperature for 1 hour, then at laboratory temperature for 30 minutes, and was then evaporated to dryness. Water (1 ml.), diethyl ether (2 ml.) and acetic acid (0.01 ml.) were added and the mixture was kept at laboratory temperature for 12 hours and then evaporated to dryness. The residue was purified by chromatography on a silica gel column using toluene as eluant and there was thus obtained benzyl 5-methyl-2-oxohexanoate as an oil.

後処理

  1. waitat laboratory temperature for 30 minutes
  2. customwas then evaporated to dryness
  3. additionWater (1 ml.), diethyl ether (2 ml.) and acetic acid (0.01 ml.) were added
  4. waitthe mixture was kept at laboratory temperature for 12 hours
  5. customevaporated to dryness
  6. customThe residue was purified by chromatography on a silica gel column

出典と根拠

ORDレコード
ord-80e098dd023b4de6a0e2fa2858024579
出典データセット
uspto-grants-1985_08
特許番号
US04533656

反応ノート

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