Formic Acid → Alpha-isopropyl-alpha-[3-[N-[2-(2-methoxyphenoxy)ethyl]-N-methylamino]propyl]-3,4-dimethoxyphenylacetonitrile

HRID 65091노트

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HRID 65091 반응식
[CH:1]([C:4]([C:22]1[CH:27]=[CH:26][C:25]([O:28][CH3:29])=[C:24]([O:30][CH3:31])[CH:23]=1)([CH2:7][CH2:8][CH2:9][NH:10][CH2:11][CH2:12][O:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[O:20][CH3:21])[C:5]#[N:6])([CH3:3])[CH3:2].C=O.[CH:34](O)=O.C(=O)([O-])[O-].[K+].[K+]>O>[CH:1]([C:4]([C:22]1[CH:27]=[CH:26][C:25]([O:28][CH3:29])=[C:24]([O:30][CH3:31])[CH:23]=1)([CH2:7][CH2:8][CH2:9][N:10]([CH2:11][CH2:12][O:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[O:20][CH3:21])[CH3:34])[C:5]#[N:6])([CH3:3])[CH3:2]

참가 물질

6

반응물 4

HCID 284Formic AcidHCID 712FormaldehydeHCID 11430Potassium CarbonateHCID 13714717HCID 13714717, 화합물

생성물 1

HCID 13714723Alpha-isopropyl-alpha-[3-[N-[2-(2-methoxyphenoxy)ethyl]-N-methylamino]propyl]-3,4-dimethoxyphenylacetonitrile

시약·촉매·용매 1

HCID 962Water용매

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온도
110 °C

실험 절차

A mixture of 2.35 g of alpha-isopropyl-alpha-[3-[N-[2-(2-methoxyphenoxy)ethyl]amino]propyl]-3,4-dimethoxyphenylacetonitrile, 8 ml of 37% formalin, and 16 ml of 90% formic acid was stirred for 1 hour at 110° C. After cooling, to the mixture were added water and potassium carbonate to make it alkaline. The solution was extracted with chloroform and the extract was washed with water, dried, and evaporated. The residue was chromatographed on silica gel using chloroform as an eluent to give 1.30 g of the desired compound as a pale yellow oil.

후처리

  1. temperatureAfter cooling, to the mixture
  2. extractionThe solution was extracted with chloroform
  3. washthe extract was washed with water
  4. customdried
  5. customevaporated
  6. customThe residue was chromatographed on silica gel

출처 및 근거

ORD 기록
ord-cc569b6f1a1549a99702b4408dea148b
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04612329

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