4-(Azidomethyl)-2,2-dimethyl-1,3-dioxolane → HCID 11497523, 화합물

HRID 2067198노트

반응식

HRID 2067198 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([F:15])=[CH:11][C:10]=2[F:16])[CH:5]=[CH:4][C:3]=1[C:17]([C:19]1[CH:24]=[C:23]([C:25]2[N:26]=[N:27][N:28]([CH2:30][CH2:31][O:32][CH:33]3[CH2:38]CC[CH2:35][O:34]3)[CH:29]=2)[CH:22]=[CH:21][C:20]=1[CH3:39])=[O:18].Cl[C:41]1C=C(NC2C=CC(F)=CC=2F)C=CC=1C(C1C=C(C#C)C=CC=1C)=O.N(CC1COC(C)(C)O1)=[N+]=[N-]>>[Cl:1][C:2]1[CH:7]=[C:6]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([F:15])=[CH:11][C:10]=2[F:16])[CH:5]=[CH:4][C:3]=1[C:17]([C:19]1[CH:24]=[C:23]([C:25]2[N:26]=[N:27][N:28]([CH2:30][CH:31]3[CH2:35][O:34][C:33]([CH3:41])([CH3:38])[O:32]3)[CH:29]=2)[CH:22]=[CH:21][C:20]=1[CH3:39])=[O:18]

참가 물질

4

반응물 3

HCID 115356024-(Azidomethyl)-2,2-dimethyl-1,3-dioxolaneHCID 11706669[2-Chloro-4-(2,4-difluoro-phenylamino)-phenyl]-(2-methyl-5-{1-[2-(tetrahydro-pyran-2-yloxy)-ethyl]-1H-[1,2,3]triazol-4-yl}-phenyl)-methanoneHCID 58677657HCID 58677657, 화합물

생성물 1

HCID 11497523HCID 11497523, 화합물

실험 절차

The reaction was carried out similarly as described in the preparation of compound 101, using compound 407 (1.37 mmol) and compound 410 (1.62 mmol). The crude product was purified by continuous gradient flash chromatography using EtOAc/petroleum ether (40-60) 20:80 to 35:65 as the eluent to afford the title compound as yellow foam. 13C NMR (DMSO-d6) δ 194.9, 158.7 (dd), 155.7 (dd), 149.4, 145.2, 139.8, 135.9, 133.7, 133.7, 131.7, 128.2, 127.1, 126.5, 126.5 (dd), 125.0, 124.2 (dd), 122.3, 114.8, 111.9 (dd), 111.8, 109.0, 105.0 (dd), 73.7, 65.8, 52.0, 26.4, 25.1, 19.4

후처리

  1. customThe crude product was purified by continuous gradient flash chromatography

출처 및 근거

ORD 기록
ord-5cda3fb023a4410ba22c304debc62a44
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08293772B2

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