Oxalyl chloride → HCID 67189596, 화합물

HRID 2240790노트

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HRID 2240790 반응식
[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]

참가 물질

4

반응물 2

HCID 65578Oxalyl chlorideHCID 11389626HCID 11389626, 화합물

생성물 1

HCID 67189596HCID 67189596, 화합물수율 57.7%

시약·촉매·용매 1

HCID 6212Chloroform용매

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온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7f3a51ba7178495fb72f249f6e86c492
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07723378B2

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