Hydrochloric Acid → HCID 59623757, 화합물

HRID 1093954노트

반응식

HRID 1093954 반응식
COC([C:5]1[S:6](=[O:21])(=[O:20])[N:7]([CH2:16][CH:17]([F:19])[F:18])[C:8]2[C:13]([C:14]=1[OH:15])=[N:12][CH:11]=[CH:10][N:9]=2)=O.Cl>C(O)C>[F:19][CH:17]([F:18])[CH2:16][N:7]1[C:8]2[C:13](=[N:12][CH:11]=[CH:10][N:9]=2)[C:14](=[O:15])[CH2:5][S:6]1(=[O:20])=[O:21]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 59623745HCID 59623745, 화합물

생성물 1

HCID 59623757HCID 59623757, 화합물수율 47.6%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
150 °C

실험 절차

To a solution of 1-(2,2-difluoro-ethyl)-4-hydroxy-2,2-dioxo-1,2-dihydro-2-λ-6-thia-1,5,8-triaza-naphthalene-3-carboxylic acid methyl ester (0.520 g) (Example 9.3) in ethanol (3 ml) was added aqueous hydrochloric acid (2M) (1 ml). The mixture was heated in a microwave for 20 minutes at 150° C. twice. The reaction mixture was concentrated to give 1-(2,2-difluoro-ethyl)-2,2-dioxo-2,3-dihydro-1H-2-λ-6-thia-1,5,8-triaza-naphthalen-4-one (0.203 g). 1H-NMR (400 MHz, CDCl3): 8.66 (d, 1H), 8.61 (d, 1H), 6.03-6.33 (m, 1H), 4.61 (s, 2H), 4.54-4.61 (m, 2H) ppm.

후처리

  1. concentrationThe reaction mixture was concentrated

출처 및 근거

ORD 기록
ord-8ebadc60d2f446738a93876208edd077
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08133849B2

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