Carbon Dioxide → HCID 67995414, 화합물

HRID 921040

반응식

HRID 921040 반응식
[C:1]([C:5]1[N:10]=[CH:9][C:8]([C:11]#[N:12])=[CH:7][N:6]=1)([CH3:4])([CH3:3])[CH3:2].Cl.Cl.[NH2:15][C:16]1[CH:17]=[N:18][C:19]([C:23]([CH3:26])([CH3:25])[CH3:24])=[CH:20][C:21]=1N.Cl.Cl.C1(N)C=CC=CC=1N.C(=O)([O-])[O-].[Na+].[Na+].C(=O)=O>C(O)C.O>[C:1]([C:5]1[N:10]=[CH:9][C:8]([C:11]2[NH:15][C:16]3[CH:17]=[N:18][C:19]([C:23]([CH3:25])([CH3:24])[CH3:26])=[CH:20][C:21]=3[N:12]=2)=[CH:7][N:6]=1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

8

반응물 5

HCID 280Carbon DioxideHCID 10340Sodium CarbonateHCID 119901,2-Phenylenediamine dihydrochlorideHCID 8177712-(Tert-butyl)pyrimidine-5-carbonitrileHCID 679950033,4-Diamino-6-tert-butylpyridine dihydrochloride

생성물 1

HCID 67995414HCID 67995414, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

실험 절차

Preparation analogous to 16), S43, using 16.1 g (100 mmol) of 2-tert-butyl-5-cyanopyrimidine [126230-72-6] and 71.4 g (300 mmol) of 3,4-diamino-6-tert-butylpyridine dihydrochloride (S50) instead of 25.9 g (100 mmol) of 2-N-pivaloylamido-3-cyano-6-tert-butylpyridine (S42) and 90.5 g (500 mmol) of o-phenylenediamine dihydrochloride [615-28-1]. After cooling, the violet melt is dissolved in a mixture of 150 ml of ethanol and 300 ml of water at elevated temperature, and a solution of 25 g of sodium carbonate in 100 ml of water is then added dropwise with vigorous stirring (note: foaming, evolution of carbon dioxide). When the addition is complete, the mixture is stirred for a further 30 min., the brown solid is then filtered off with suction, washed three times with 100 ml of water each time and dried in vacuo. Yield: 23.8 g (77 mmol), 77%. Purity: >95% according to 1H-NMR.

후처리

  1. customPreparation analogous to 16), S43
  2. temperatureAfter cooling
  3. additionWhen the addition
  4. filtrationthe brown solid is then filtered off with suction
  5. washwashed three times with 100 ml of water each time
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-5e49d604c9bd434f8499cee66314e496
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09273080B2

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