Triethylamine → HCID 178490640, 화합물

HRID 538773노트

반응식

HRID 538773 반응식
[C:1]([O:4][C:5]1([CH2:9][N:10]2[CH:14]=[C:13]([C:15]([CH3:18])([CH3:17])[CH3:16])[S:12]/[C:11]/2=[N:19]\[C:20]([C:22]2[CH:27]=[C:26]([Cl:28])[CH:25]=[CH:24][C:23]=2[O:29][CH3:30])=S)[CH2:8][CH2:7][CH2:6]1)(=[O:3])[CH3:2].C(N(CC)CC)C.[N:38]#[C:39][NH2:40]>C(#N)C.[Hg](OC(C)=O)OC(C)=O>[C:1]([O:4][C:5]1([CH2:9][N:10]2[CH:14]=[C:13]([C:15]([CH3:18])([CH3:17])[CH3:16])[S:12]/[C:11]/2=[N:19]\[C:20]([C:22]2[CH:27]=[C:26]([Cl:28])[CH:25]=[CH:24][C:23]=2[O:29][CH3:30])=[N:40][C:39]#[N:38])[CH2:8][CH2:7][CH2:6]1)(=[O:3])[CH3:2]

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 9864CyanamideHCID 178490712HCID 178490712, 화합물

생성물 1

HCID 178490640HCID 178490640, 화합물수율 77%

시약·촉매·용매 2

HCID 16683746Diacetyloxymercury촉매HCID 6342Acetonitrile용매

실험 절차

The product of Example 27D (1.2 g, 2.6 mmol), triethylamine (1.4 mL, 10 mmol), cyanamide (0.32 g, 7.7 mmol) and Hg(OAc)2 (1.6 g, 5.1 mmol) in acetonitrile (20 mL) were processed as described in Example 16E to provide the title compound (0.93 g, 2.0 mmol, 77% yield). 1H NMR (300 MHz, CDCl3) δ ppm 1.38 (s, 9H), 1.73-1.96 (m, 2H), 1.99 (s, 3H), 2.22-2.46 (m, 4H), 3.91 (s, 3H), 4.76 (s, 2H), 6.63 (s, 1H), 6.94 (d, J=8.8 Hz, 1H), 7.31-7.39 (m, 2H); MS (DCI/NH3) m/z 475 (M+H)+. Anal. calculated for C23H27 ClN4O3S: C, 58.16; H, 5.73; N, 11.80. Found: C, 58.16; H, 5.66; N, 11.85.

출처 및 근거

ORD 기록
ord-b116de3c95f0426787a35b284eaad6cb
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08865753B2

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