Acetic Acid → 4-Chloro-2,5-diamino-6-neopentyl-pyrimidine

HRID 1181213노트

반응식

HRID 1181213 반응식
[NH2:1][C:2]1[N:7]=[C:6]([Cl:8])[CH:5]=[C:4]([CH2:9][C:10]([CH3:13])([CH3:12])[CH3:11])[N:3]=1.C([O-])(=O)C.[Na+].C(O)(=O)C.F[P-](F)(F)(F)(F)F.ClC1C=CC([N+:37]#N)=CC=1>O.C(O)C.O.[Zn]>[Cl:8][C:6]1[C:5]([NH2:37])=[C:4]([CH2:9][C:10]([CH3:13])([CH3:12])[CH3:11])[N:3]=[C:2]([NH2:1])[N:7]=1

참가 물질

8

반응물 4

HCID 176Acetic Acid2회HCID 517045Sodium AcetateHCID 2723983Benzenediazonium, 4-chloro-, hexafluorophosphate(1-) (1:1)HCID 222749822-Amino-4-chloro-6-neopentylpyrimidine

생성물 1

HCID 222749464-Chloro-2,5-diamino-6-neopentyl-pyrimidine

시약·촉매·용매 3

HCID 23994Zinc촉매HCID 962Water용매HCID 19096565Water ethanol용매

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온도
25 °C

실험 절차

A mixture of 2-amino-4-chloro-6-neopentylpyrimidine (1 mmol), sodium acetate (14 mmol), acetic acid (86 mmol), and 4-chlorobenzene-diazonium hexafluorophosphate (1.15 mmol) in water was stirred at 25° C. for 12 h. Extraction and evaporation gave a yellow solid which was treated with zinc dust (10 mmol) and acetic acid (5.54 mmol) in EtOH-H2O at 80° C. for 1 h. Extraction and chromatography gave 4-chloro-2,5-diamino-6-neopentyl-pyrimidine as a yellow solid. TLC: Rf=0.25, 50% EtOAc-hexane.

후처리

  1. extractionExtraction and evaporation
  2. customgave a yellow solid which
  3. extractionExtraction and chromatography

출처 및 근거

ORD 기록
ord-09ffa72cb21047dd815f426161ecb07a
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07285543B2

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