Oxalyl chloride → HCID 67189596, 화합물

HRID 1665928노트

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HRID 1665928 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-4b3007dc98f84138b065c58d06cdb653
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08039644B2

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