Water → N-cyclopropylpyridin-4-amine

HRID 1763160노트

반응식

HRID 1763160 반응식
Cl[C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.[CH:15]1([NH2:18])[CH2:17][CH2:16]1.O>CN(C=O)C>[CH:15]1([NH:18][C:2]2[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=2)[CH2:17][CH2:16]1

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 122884-ChloropyridineHCID 69828Cyclopropylamine

생성물 1

HCID 19854218N-cyclopropylpyridin-4-amine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a magnetically stirred, 25° C. solution of 2.3 g (0.006 mol) of product of Step A and 0.71 g (0.007 mol) of triethylamine in 40 ml of DMF was added dropwise 0.38 g (0.007 mol) of cyclopropylamine. After 18 hours the reaction mixture was poured into H2O and extracted with diethyl ether. The ether phase was washed with H2O, and dried (MgSO4). The dry ether phase was concentrated in vacuo to 1.95 g of a brown solid. The crude was recrystallized from hexane/EtOAc affording 1.2 g (50%) of product as a beige solid; mp 111°-112° C.

후처리

  1. extractionextracted with diethyl ether
  2. washThe ether phase was washed with H2O
  3. dry with materialdried (MgSO4)
  4. concentrationThe dry ether phase was concentrated in vacuo to 1.95 g of a brown solid
  5. customThe crude was recrystallized from hexane/EtOAc affording 1.2 g (50%) of product as a beige solid

출처 및 근거

ORD 기록
ord-d81f1813a41742749d5ec440ac635f4c
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04835279

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