Ammonia → HCID 385198, 화합물

HRID 1421876노트

반응식

HRID 1421876 반응식
[NH2:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][C:10]2([CH2:14][OH:15])[CH2:13][CH2:12][CH2:11]2)[CH:5]=[CH:4][N:3]=1.C([O-])(=O)C.[Na+].[Br:21]Br.N>C(O)(=O)C.O>[NH2:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][C:10]2([CH2:14][OH:15])[CH2:13][CH2:12][CH2:11]2)[C:5]([Br:21])=[CH:4][N:3]=1

참가 물질

7

반응물 4

HCID 222AmmoniaHCID 24408BromineHCID 385194HCID 385194, 화합물HCID 517045Sodium Acetate

생성물 1

HCID 385198HCID 385198, 화합물수율 72.4%

시약·촉매·용매 2

HCID 176Acetic Acid용매2회HCID 962Water용매

반응 조건

온도
110 °C

실험 절차

To 2-amino-4-[[(1-hydroxymethyl-1-cyclobutyl)methyl]amino]pyrimidine (0.21 g, 1.0 mmol) was added acetic acid (3 ml) and the mixture was heated to 110° C. Sodium acetate 3 hydrate (0.18 g) was added and bromine (60 μl) dissolved in acetic acid (0.5 ml) was dropwise added at 70° C. After cooling, water was added to the reaction mixture and the mixture was neutralized with aqueous ammonia under ice-cooling, extracted with ethyl acetate and dried over anhydrous magnesium sulfate. The solvent was distilled away under reduced pressure and the residue was recrystallized from acetone to give colorless prism crystals (0.21 g, 72.4%), m.p. 156-158° C. (acetone).

후처리

  1. additionwas dropwise added at 70° C
  2. temperatureAfter cooling
  3. temperaturecooling
  4. extractionextracted with ethyl acetate
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled away under reduced pressure
  7. customthe residue was recrystallized from acetone

출처 및 근거

ORD 기록
ord-e789c5d0393a40449349d26c8ae6d3d4
출처 데이터셋
uspto-grants-2000_06
특허 번호
US06080750

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