Acetyl chloride → HCID 85826160、化合物

HRID 2064673ノート

反応式

HRID 2064673 の反応式
[Cl-].[Mg+2].[Cl-].[CH2:4]([O:6][C:7](=[O:17])[CH2:8][C:9](=[O:16])[CH2:10][O:11][C:12]([CH3:15])([CH3:14])[CH3:13])[CH3:5].[C:18](Cl)(=[O:20])[CH3:19].[Cl-].[NH4+]>ClCCl.N1C=CC=CC=1>[CH2:4]([O:6][C:7](=[O:17])[CH:8]([C:18](=[O:20])[CH3:19])[C:9](=[O:16])[CH2:10][O:11][C:12]([CH3:13])([CH3:15])[CH3:14])[CH3:5]

参加物

7

反応物 4

HCID 6367Acetyl chlorideHCID 25517Ammonium ChlorideHCID 5360315Magnesium ChlorideHCID 11790264Ethyl 4-(tert-butoxy)-3-oxobutanoate

生成物 1

HCID 85826160HCID 85826160、化合物

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

A suspension of dry magnesium chloride (0.471 g) in dichloromethane (6 ml) was treated with 4-tert-butoxy-3-oxo-butyric acid ethyl ester [1.00 g, Reference Example 43]. This mixture was cooled to 0° C., then treated with pyridine (0.80 ml), then stirred for 15 minutes at 0° C. and then treated with acetyl chloride (0.352 ml). After stirring for a further 15 minutes at 0° C. and then for 1 hour at ambient temperature the reaction mixture was treated with saturated aqueous ammonium chloride solution and then extracted twice with ethyl acetate. The combined extracts were dried over magnesium sulfate and then evaporated to yield 2-acetyl-4-tert-butoxy-3-oxo-butyric acid ethyl ester (1.15 g) as a yellow oil which was used without further purification. LC-MS (METHOD B): RT=3.16 minutes; 243 (M−H)−.

後処理

  1. stirringAfter stirring for a further 15 minutes at 0° C.
  2. extractionextracted twice with ethyl acetate
  3. dry with materialThe combined extracts were dried over magnesium sulfate
  4. customevaporated

出典と根拠

ORDレコード
ord-911552e7b9464f0991adb0a205215e01
出典データセット
uspto-grants-2012_10
特許番号
US08288425B2

反応ノート

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