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Triethylamine → HCID 22011937, 화합물

HRID 1532957
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HRID 1532957 반응식
Cl[C:2]1[C:7]([Cl:8])=[C:6]([CH2:9][CH3:10])[N:5]=[CH:4][N:3]=1.[NH2:11][CH:12]1[CH2:16][O:15][CH:14]([CH3:17])[CH2:13]1.CC1CC(O)CO1.C(N(CC)CC)C>O>[Cl:8][C:7]1[C:2]([NH:11][CH:12]2[CH2:16][O:15][CH:14]([CH3:17])[CH2:13]2)=[N:3][CH:4]=[N:5][C:6]=1[CH2:9][CH3:10]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 347412,5-Anhydro-1,3-dideoxypentitolHCID 111376684,5-Dichloro-6-ethylpyrimidineHCID 220119415-Methyloxolan-3-amine

생성물 1

HCID 22011937HCID 22011937, 화합물

시약·촉매·용매 1

HCID 962Water용매

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온도
85 °C

실험 절차

1.5 g of 4,5-dichloro-6-ethylpyrimidine (8.5 mmol), 0.86 g (8.5 mmol) of 4-amino-2-methyltetrahydrofuran (prepared from 2-methyltetrahydrofuran4-ol analogously to the route given for Example A) and 2 ml (14 mmol) of triethylamine were heated for 6 hours at 85° C. After cooling, the mixture was diluted with water and extracted with ether, and the organic phase was washed with saturated NaCl solution. After drying and concentrating, the residue was purified by column chromatography using petroleum ether/ethyl acetate (8:2, 7:3). This gave 1.73 g (84% of theory) of a colorless oil (diastereomers 2:1).

후처리

  1. temperatureAfter cooling
  2. extractionextracted with ether
  3. washthe organic phase was washed with saturated NaCl solution
  4. customAfter drying
  5. concentrationconcentrating
  6. customthe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-ebbd76da17b9409793fced008f75a2ea
출처 데이터셋
uspto-grants-2001_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06207668B1

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