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HCID 69312679, 화합물 → HCID 15565856, 화합물

HRID 902519
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HRID 902519 반응식
[CH2:1]([O:3][C:4]([C:6]1[C:11](=[O:12])[N:10](CC2C=CC(OC)=CC=2)[C:9]2[CH:22]=[CH:23][S:24][C:8]=2[C:7]=1[Cl:25])=[O:5])[CH3:2]>C(O)(C(F)(F)F)=O>[CH2:1]([O:3][C:4]([C:6]1[C:11](=[O:12])[NH:10][C:9]2[CH:22]=[CH:23][S:24][C:8]=2[C:7]=1[Cl:25])=[O:5])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 69312679HCID 69312679, 화합물

생성물 1

HCID 15565856HCID 15565856, 화합물수율 99.9%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

A solution of 7-chloro-4-(4-methoxybenzyl)-5-oxo-4,5-dihydro-thieno[3,2-b]pyridine-6-carboxylic acid ethyl ester (55) (10.40 g, 27.5 mmol) in neat TFA was heated at 70° C. under argon for 36 h. The solution was cooled and poured into ice water. The solids formed were filtered, washed by water, and dried to yield 7.08 g (99%) of 7-chloro-5-oxo-4,5-dihydro-thieno[3,2-b]pyridine-6-carboxylic acid ethyl ester as white solids. MP 206° C.; 1H NMR (400 MHz, DMSO-d6) δ 1.28 (t, J=7.2 Hz, 3H), 4.29 (q, J=7.2 Hz, 2H), 7.10 (d, J=5.2 Hz, 1H), 8.13 (d, J=5.2 Hz, 1H) ppm; MS m/z=240 amu (M++1).

후처리

  1. temperatureThe solution was cooled
  • customThe solids formed
  • filtrationwere filtered
  • washwashed by water
  • customdried
  • 출처 및 근거

    ORD 기록
    ord-c856f620fd314dba982d8c7be1b11ad7
    출처 데이터셋
    uspto-grants-2008_04
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US07365200B2

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