Chlorosulfonic acid → HCID 178524660, 화합물

반응식

[OH:1][C:2]1[N:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[Cl:11][S:12](O)(=[O:14])=[O:13]>>[Cl:11][S:12]([C:8]1[CH:9]=[N:10][C:2]([OH:1])=[C:3]([CH:7]=1)[C:4]([OH:6])=[O:5])(=[O:14])=[O:13]

참가 물질

반응물 2

HCID 24638Chlorosulfonic acid

HCID 178418543HCID 178418543, 화합물

생성물 1

HCID 178524660HCID 178524660, 화합물수율 44%

반응 조건

온도: 160 °C

실험 절차

2-Hydroxynicotinic acid (10.0 g, 71.8 mmol) was dissolved in 25 ml of chlorosulfonic acid and heated to 160° C. overnight. After cooling the reaction was slowly poured into ice and stirred in an ice bath until a white precipitate formed. The solid was filtered off and dried under vacuum to afford 7.55 g of 5-(chlorosulfonyl)-2-hydroxynicotinic acid (44% yield). 1H NMR (300 MHz, DMSO-d6) δ ppm 7.9 (dd, J=2.5, 0.7 Hz, 1H) 8.4 (dd, J=2.6, 0.7 Hz, 1H).

후처리

temperatureAfter cooling the reaction
additionwas slowly poured into ice
customformed
filtrationThe solid was filtered off
customdried under vacuum

출처 및 근거

ORD 기록: ord-7124389b873741a48a2103f353314827
출처 데이터셋: uspto-grants-2010_01
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US07645771B2

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