Bromine → Methyl 2,3-methylenedioxy-4-methoxy-5-bromobenzoate

HRID 976255노트

반응식

HRID 976255 반응식
[CH2:1]1[O:13][C:12]2[C:3](=[C:4]([CH:9]=[CH:10][C:11]=2[O:14][CH3:15])[C:5]([O:7][CH3:8])=[O:6])[O:2]1.[Br:16]Br>C(Cl)(Cl)Cl>[CH2:1]1[O:13][C:12]2[C:3](=[C:4]([CH:9]=[C:10]([Br:16])[C:11]=2[O:14][CH3:15])[C:5]([O:7][CH3:8])=[O:6])[O:2]1

참가 물질

4

반응물 2

HCID 24408BromineHCID 19967040HCID 19967040, 화합물

생성물 1

HCID 13170923Methyl 2,3-methylenedioxy-4-methoxy-5-bromobenzoate수율 93.2%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

Compound 122 (5.56 g, 25.6 mmol) was dissolved in anhydrous chloroform. Bromine (4.5 g, 28.5 mmol) was added dropwise over 2 hours at 5°-8° C. Then the mixture was maintained for an additional 2 hours at the same temperature. After the usual workup, 6.9 g of white solid 123 was obtained (88% yield). m.p. 165°-6° C. (crystallized from ethyl acetate). IR cm-1 1710 (s, C=O), 1425, 1400 (s, C--O); MS m/z (%): 288 (M+, 100), 290 (M+2, 96); 1H NMR δ ppm 3.91 (s, 3H, OCH3), 4.14 (s, 3H, ArOCH3), 6.10 (s, 2H, OCH2O), 7.65 (s, 1H, 6-ArH); Anal. (C10H9O5Br) C, H, Br.

후처리

  1. temperatureThen the mixture was maintained for an additional 2 hours at the same temperature

출처 및 근거

ORD 기록
ord-ed5d5bab11e248d3b87016569709c47d
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05612341

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