Trimethyl orthoformate → HCID 66985986, 화합물

HRID 1622112노트

반응식

HRID 1622112 반응식
[Br:1][C:2]1[C:3]([O:10][CH3:11])=[C:4]([CH:7]=[CH:8][CH:9]=1)C=O.CO[CH:14]([O:17][CH3:18])[O:15][CH3:16].ClS(O)(=O)=O>CO>[Br:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:4]([CH:14]([O:15][CH3:16])[O:17][CH3:18])[C:3]=1[O:10][CH3:11]

참가 물질

5

반응물 3

HCID 9005Trimethyl orthoformateHCID 24638Chlorosulfonic acidHCID 110638083-Bromo-2-methoxybenzaldehyde

생성물 1

HCID 66985986HCID 66985986, 화합물수율 81%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

3-Bromo-2-methoxybenzaldehyde (28 g, 130 mmol) was combined with trimethylorthoformate (27.5 g, 28.6 mL, 260 mmol) in methanol (150 mL) and then chlorosulfonic acid (0.5 mL) was added dropwise to the mixture. The mixture was stirred for 3 hours and then concentrated by rotoevaporation. The residue was partitioned between ethyl ether and 5% aqueous sodium bicarbonate and the organic layer was separated, washed with water and brine, dried over sodium sulfate and concentrated to give 1-bromo-3-dimethoxymethyl-2-methoxybenzene (27.5 g).

후처리

  1. concentrationconcentrated by rotoevaporation
  2. customThe residue was partitioned between ethyl ether and 5% aqueous sodium bicarbonate
  3. customthe organic layer was separated
  4. washwashed with water and brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-eba316e2bce745b8897eb65493d2c9a0
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08778625B2

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