(E)-tert-Butyl 3-(6-acetyl-3-chloro-2-fluorophenyl)acrylate → HCID 66698622, 화합물

HRID 1054130노트

반응식

HRID 1054130 반응식
[C:1]([C:4]1[C:9](/[CH:10]=[CH:11]/[C:12]([O:14]C(C)(C)C)=[O:13])=[C:8]([F:19])[C:7]([Cl:20])=[CH:6][CH:5]=1)(=[O:3])[CH3:2]>C(Cl)Cl.C(O)(C(F)(F)F)=O>[C:1]([C:4]1[C:9](/[CH:10]=[CH:11]/[C:12]([OH:14])=[O:13])=[C:8]([F:19])[C:7]([Cl:20])=[CH:6][CH:5]=1)(=[O:3])[CH3:2]

참가 물질

4

반응물 1

HCID 66698573(E)-tert-Butyl 3-(6-acetyl-3-chloro-2-fluorophenyl)acrylate

생성물 1

HCID 66698622HCID 66698622, 화합물수율 97%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid용매

실험 절차

A solution of Intermediate 12D (25 g, 84 mmol) in DCM (330 mL) and TFA (330 mL) was stirred at rt. After 1.5 h, the solvent was concentrated to give Intermediate 12 (19.5 g, 97.0% yield) as a white solid. 1H NMR (400 MHz, DMSO-d6) δ: 12.69 (bs, 1H), 7.80-7.76 (m, 2H), 7.62 (d, J=12.1 Hz, 1H), 6.30 (dd, J=2.4, 2.0 Hz, 1H), 2.6 (s, 3H) ppm. MS (ESI) m/z: 241 (M−H)+.

후처리

  1. concentrationthe solvent was concentrated

출처 및 근거

ORD 기록
ord-f26e720174874bacbeb0bc6fb2e4ffd6
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09394276B2

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