1,2-Dichloroethane → 4-(Dimethylamino)but-2-enoic acid

HRID 1027841노트

반응식

HRID 1027841 반응식
Br[CH2:2][CH:3]=[CH:4][C:5]([OH:7])=[O:6].[CH3:8][NH:9][CH3:10].C(Cl)CCl>C1COCC1.CN(C=O)C>[CH3:8][N:9]([CH3:10])[CH2:2][CH:3]=[CH:4][C:5]([OH:7])=[O:6]

참가 물질

6

반응물 3

HCID 111,2-DichloroethaneHCID 674DimethylamineHCID 841404-Bromo-2-butenoic acid

생성물 1

HCID 533952454-(Dimethylamino)but-2-enoic acid수율 40%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8028Tetrahydrofuran용매

실험 절차

100 mg of 4-dimethylamino-2-butenoic acid (0.63 mmol) which was prepared by reaction between 4-bromo-2-butenoic acid and dimethylamine in THF, was added in 2 ml DMF and 185 mg of 4 (0.53 mmol) was added followed by 0.6 mmol EDC. The mixture was stirred over night at room temperature and the final product was purified by preparative HPLC to give 120 mg product as light yellow solid, yield 40%. HPLC-MS: m/z: 496 [M+1]+.

후처리

  1. customthe final product was purified by preparative HPLC

출처 및 근거

ORD 기록
ord-92407dcdf20447158864ba06ae12199a
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08735409B2

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