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[C:1]([Cl:4])(Cl)=[O:2].[C:5]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15]O)=[CH:11][CH:10]=1)(=[O:7])[CH3:6]>C1(C)C=CC=CC=1>[C:5]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][C:1]([Cl:4])=[O:2])=[CH:11][CH:10]=1)(=[O:7])[CH3:6]참가 물질
4
실험 절차
To a solution of phosgene in toluene (20% w/w, 2.2 mL, 4.2 mmol), cooled in an ice bath, was added dropwise a solution of 60 (321 mg, 1.9 mmol) in 2 mL of toluene. The mixture was stirred in the same bath, which was left to come to room temperature on its own. After 18 h, the mixture was concentrated in vacuo to give 61, which was used in the next step without further purification. 1H NMR (400 MHz, CDCl3) δ 2.30 (s, 3H), 5.28 (s, 2H), 7.13 (d, J=8.6 Hz, 2H), 7.42 (d, J=8.7 Hz, 2H).
후처리
- waitwas left
- customto come to room temperature on its
- concentrationthe mixture was concentrated in vacuo
출처 및 근거
- ORD 기록
- ord-92490217d32c40b8aa54f432ecaf61a4
- 출처 데이터셋
- uspto-grants-2013_09
- 특허 번호
- US08524691B2
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