Diethylamine → HCID 70979643, 화합물

HRID 1468649노트

반응식

HRID 1468649 반응식
Br[CH2:2][CH2:3][O:4][C:5]1[CH:10]=[C:9]([S:11]([CH3:14])(=[O:13])=[O:12])[CH:8]=[C:7]([F:15])[CH:6]=1.[CH2:16]([NH:18][CH2:19][CH3:20])[CH3:17]>C(O)C>[CH2:16]([N:18]([CH2:19][CH3:20])[CH2:2][CH2:3][O:4][C:5]1[CH:10]=[C:9]([S:11]([CH3:14])(=[O:13])=[O:12])[CH:8]=[C:7]([F:15])[CH:6]=1)[CH3:17]

참가 물질

4

반응물 2

HCID 8021DiethylamineHCID 86717739HCID 86717739, 화합물

생성물 1

HCID 70979643HCID 70979643, 화합물수율 61.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Preparation according to Example 1 but performed in one portion: 1-(2-bromoethoxy)-3-fluoro-5-methylsulfonyl-benzene (0.5 g, 1.68 mmol) and di-ethylamine (1.39 ml, 13.46 mmol) in ethanol (4 ml). Purification by flash column chromatography (ethyl acetate/methanol, 1:0 to 1:1) gave the title compound (300 mg, 61.6%). The amine was converted to the hydrochloric acid salt and re-crystallized from methanol/diethyl ether: M.p. 172.3° C. MS m/z (relative intensity, 70 eV) 289 (M+, 1), 274 (6), 87 (6), 86 (bp), 58 (5).

후처리

  1. customPreparation
  2. customPurification by flash column chromatography (ethyl acetate/methanol, 1:0 to 1:1)

출처 및 근거

ORD 기록
ord-a403d57cf13d4f10ade6bba55295f3db
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09006227B2

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