Water → HCID 21474587、化合物

HRID 2294542ノート

反応式

HRID 2294542 の反応式
[CH3:1][C:2]1([CH3:19])[CH2:11][CH2:10][C:9]([CH3:13])([CH3:12])[C:8]2[CH:7]=[C:6]([C:14](=[O:18])[C:15]([OH:17])=[O:16])[CH:5]=[CH:4][C:3]1=2.[CH2:20]1COCC1.C([Mg]I)C.O>C(OCC)C>[OH:18][C:14]([C:6]1[CH:5]=[CH:4][C:3]2[C:2]([CH3:19])([CH3:1])[CH2:11][CH2:10][C:9]([CH3:12])([CH3:13])[C:8]=2[CH:7]=1)([CH3:20])[C:15]([OH:17])=[O:16]

参加物

6

反応物 4

HCID 962WaterHCID 8028TetrahydrofuranHCID 12051800HCID 12051800、化合物HCID 178461634HCID 178461634、化合物

生成物 1

HCID 21474587HCID 21474587、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

3.1 g (12 mmol) of 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthylglyoxylic acid and 50 ml of THF are introduced into a three-necked flask. At 0° C. and under a stream of nitrogen, 16 ml (48 mmol) of a solution of ethylmagnesium iodide in ethyl ether (3M) are added dropwise and the mixture is stirred at room temperature for four hours. The reaction medium is poured into water, the mixture is extracted with ethyl ether and the organic phase is separated after settling has taken place, then dried over magnesium sulphate and evaporated. The residue obtained is purified by chromatography on a silica column and eluted with a mixture of dichloromethane and ethyl ether (20:80). After evaporation of the solvents, 2.6 g (79%) of the expected product, melting point 168°-169° C., are collected.

後処理

  1. extractionthe mixture is extracted with ethyl ether
  2. customthe organic phase is separated after settling
  3. dry with materialdried over magnesium sulphate
  4. customevaporated
  5. customThe residue obtained
  6. customis purified by chromatography on a silica column
  7. washeluted with a mixture of dichloromethane and ethyl ether (20:80)
  8. customAfter evaporation of the solvents, 2.6 g (79%) of the expected product, melting point 168°-169° C.
  9. customare collected

出典と根拠

ORDレコード
ord-a3c66a906def47a788029a1f7f309aa1
出典データセット
uspto-grants-1997_11
特許番号
US05688817

反応ノート

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