Oxalyl chloride → 5-(Benzyloxy)pentanoyl chloride
반응식
[CH2:1]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]([OH:15])=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(Cl)(=O)C([Cl:19])=O>C1C=CC=CC=1>[CH2:1]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]([Cl:19])=[O:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1참가 물질
4
실험 절차
To a solution of the acid 29 (4.98 g, 24 mmol) in dry benzene (40 ml), was added oxalyl chloride (2.5 ml, 28.8 mmol, 1.2 equiv) dropwise. A drying tube was placed on the flask and the reaction was stirred for 90 min at room temperature. The reaction was concentrated in vacuo and used directly in the next step: 1H NMR (400 MHz, CDCl3) δ 7.38-7.27 (m, 5H), 4.50 (s, 2H), 3.51-3.40 (t, 3J=6.4 Hz, 2H), 2.95-2.90 (t, 3J=7.2 Hz, 3H), 1.87-1.78 (m, 2H), 1.71-1.63 (m, 2H); 13C NMR (75 MHz, CDCl3) δ 173.958, 138.519, 128.949, 128.787, 128.630, 127.862, 73.197, 69.551, 47.032, 28.618, 22.329.
후처리
- customA drying tube was placed on the flask
- concentrationThe reaction was concentrated in vacuo
출처 및 근거
- ORD 기록
- ord-1d18e44234d34735bf07cd7d56a45342
- 출처 데이터셋
- uspto-grants-2011_02
- 특허 번호
- US07893268B2
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