Triphenylphosphine → HCID 178443932, 화합물
반응식
CCOC(/N=N/C(OCC)=O)=O.[F:13][C@H:14]([CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH3:22])[CH2:15][OH:16].[F:23][C:24]1[C:29]([F:30])=[C:28]([CH2:31][CH2:32][C@H:33]2[CH2:38][CH2:37][C@H:36]([CH2:39][CH2:40][CH2:41][CH2:42][CH3:43])[CH2:35][CH2:34]2)[CH:27]=[CH:26][C:25]=1[C:44]1[N:49]=[CH:48][C:47](O)=[CH:46][N:45]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.FC1C(F)=C(CCCCC)C=CC=1C1N=CC(OC[C@H](F)CCCCCC)=CN=1>C1COCC1>[F:23][C:24]1[C:29]([F:30])=[C:28]([CH2:31][CH2:32][C@H:33]2[CH2:34][CH2:35][C@H:36]([CH2:39][CH2:40][CH2:41][CH2:42][CH3:43])[CH2:37][CH2:38]2)[CH:27]=[CH:26][C:25]=1[C:44]1[N:45]=[CH:46][C:47]([O:16][CH2:15][C@H:14]([F:13])[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH3:22])=[CH:48][N:49]=1참가 물질
실험 절차
--Quantities: DEAD (448 mg, 2.58 mmol) in THF (3 ml), (R)-(+)-2-fluorooctanol (379 mg, 2.58 mmol), hydroxypyrimidine 48 (1.0 g, 2.58 mmol), triphenylphosphine (676 mg, 2.58 mmol). The experimental procedure was as described for compound 34. The crude product was purified by flash chromatography (5 to 7% ethyl acetate-light petroleum) to give the 2-fluorooctyloxypyrimidine 49 (820 mg, 61%) (from EtOH), transitions/° C. K 102.2 N* 128.3 I; [α]D26 -2.4° (c 2.0 in CHCl3); νmax /cm-1 (KBr) 2920, 2845, 1540, 1460, 1435s, 1285 1085, and 900; δ 0.80-1.03 (10H, m), 1.06-1.45 (16H, m), 1.55 (4H, m), 1.82 (6H, m), 2.71 (2H, t J 8, ArCH2), 4.22 (2H, dd, 3JHF 22 and J 4, OCH2), 4.86 (1H, d of sext, 2JHF 48 and J 4, CHF), 7.01 (1H, ddd, J 7.5, 7 and 1.5, 5'-H), 7.67 (1H, ddd, J 7.5, 7 and 1.5, 5'-H) and 8.53 (2H, s, 4- and 6-H); m/z 518 (M+), 489, 475, 461, 447, 365 and 353.
후처리
- customThe crude product was purified by flash chromatography (5 to 7% ethyl acetate-light petroleum)
출처 및 근거
- ORD 기록
- ord-baacf50b1cae426f934ced85b5e9df81
- 출처 데이터셋
- uspto-grants-1999_11
- 특허 번호
- US05986096
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