Triethylamine → HCID 22011946, 화합물

HRID 1532958

반응식

HRID 1532958 반응식
Cl[C:2]1[C:7]([O:8][CH3:9])=[C:6]([CH2:10][O:11][CH3:12])[N:5]=[CH:4][N:3]=1.[NH2:13][CH:14]1[CH2:18][S:17][CH:16]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH2:15]1.C1(C2CC(=O)CS2)C=CC=CC=1.C(N(CC)CC)C>O>[CH3:9][O:8][C:7]1[C:2]([NH:13][CH:14]2[CH2:18][S:17][CH:16]([C:19]3[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=3)[CH2:15]2)=[N:3][CH:4]=[N:5][C:6]=1[CH2:10][O:11][CH3:12]

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 124137022-Phenyl-4-oxo-tetrahydrothiopheneHCID 152793504-Chloro-5-methoxy-6-(methoxymethyl)pyrimidineHCID 220119364-Amino-2-phenyltetrahydrothiophene

생성물 1

HCID 22011946HCID 22011946, 화합물

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
85 °C

실험 절차

1.6 g (8.5 mmol) of 4-chloro-5-methoxy-6-methoxymethylpyrimidine, 1.5 g (8.5 mmol) of 4-amino-2-phenyltetrahydrothiophene (prepared from 2-phenyl-4-oxo-tetrahydrothiophene (cf. D. N. Reinhard, W. P. Trompenaars, I. Geevers, Synthesis 1978, 368) analogously to the route given in Example B) and 2 ml (14 mmol) of triethylamine were heated for 24 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 (9:1). This gave 1.18 g (42% of theory) of a pale yellow syrup.

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-f09260a59f884186b0b403e683e853c8
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06207668B1

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