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Water → HCID 89704808, 화합물

HRID 928994
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HRID 928994 반응식
[NH2:1][C:2]1[C:11]([SH:12])=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([NH:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=2[F:20])[C:3]=1[F:21].[CH3:22]C1C=CC(S(O)(=O)=O)=CC=1.O>C(OC)(OC)OC>[F:21][C:3]1[C:2]2[N:1]=[CH:22][S:12][C:11]=2[CH:10]=[C:5]([C:6]([O:8][CH3:9])=[O:7])[C:4]=1[NH:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[F:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 6101p-Toluenesulfonic acidHCID 89704800HCID 89704800, 화합물

생성물 1

HCID 89704808HCID 89704808, 화합물수율 85.1%

시약·촉매·용매 1

HCID 9005Trimethyl orthoformate용매

실험 절차

To a solution of methyl 4-amino-3-fluoro-2-((2-fluorophenyl)amino)-5-mercaptobenzoate in trimethyl orthoformate (50 mL) was added p-TsOH (0.61 g, 3.17 mmol). The reaction mixture was stirred for 1 h and treated with water (100 mL). The precipitate was filtered off and the filter cake was washed with water to afford the desired product (pale yellow solid, 8.64 g, 85.1% yield for two steps). 1H NMR (400 MHz, CDCl3): δ 9.13 (s, 1H), 8.68 (s, 1H), 8.46 (s, 1H), 7.10 (m, 1H), 7.01 (m, 1H), 6.92 (s, 2H), 3.97 (s, 3H).

후처리

  1. filtrationThe precipitate was filtered off
  2. washthe filter cake was washed with water

출처 및 근거

ORD 기록
ord-6a88660919534373bbaeca9588c60e94
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09290468B2

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