Oxalyl chloride → HCID 67189596、化合物

HRID 2240790ノート

反応式

HRID 2240790 の反応式
[C:1]([CH:4]1[CH2:9][C:8]([CH3:11])([CH3:10])[CH2:7][CH2:6][C:5]1=[O:12])(=O)[CH3:2].C(Cl)(=O)C([Cl:16])=O>C(Cl)(Cl)Cl>[Cl:16][C:1](=[C:4]1[CH2:9][C:8]([CH3:11])([CH3:10])[CH2:7][CH2:6][C:5]1=[O:12])[CH3:2]

参加物

4

反応物 2

HCID 65578Oxalyl chlorideHCID 11389626HCID 11389626、化合物

生成物 1

HCID 67189596HCID 67189596、化合物収率 57.7%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
60 °C

実験手順

At 0° C., a solution of 2-acetyl-4,4-dimethyl-cyclohexanone (5.00 g, 29.7 mmol) in chloroform (15 mL) is treated with oxalyl chloride (7.54 g, 59.4 mmol). The mixture is heated to 60° C. and stirred for 15 min before it is poured onto water. The organic phase is separated, washed with sat. aq. NaHCO3 solution and brine, dried over MgSO4 and evaporated to dryness to give crude 2-(1-chloro-ethylidene)-4,4-dimethyl-cyclohexanone (3.2 g, containing regio-isomer) as a brown oil, LC-MS: tR=1.00 min.

後処理

  1. additionis poured onto water
  2. customThe organic phase is separated
  3. washwashed with sat. aq. NaHCO3 solution and brine
  4. dry with materialdried over MgSO4
  5. customevaporated to dryness

出典と根拠

ORDレコード
ord-7f3a51ba7178495fb72f249f6e86c492
出典データセット
uspto-grants-2010_05
特許番号
US07723378B2

反応ノート

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