Hydrochloric Acid → HCID 69073584、化合物

HRID 216155

反応式

HRID 216155 の反応式
[Cl:1]C1C=C(Cl)C=CC=1CCNC1N=C(OC)N=C(C2C=C(O)C=CC=2)C=1.[N+](C1C=CC(CCN)=CC=1)([O-])=O.[Cl:39][C:40]1[CH:45]=[CH:44][CH:43]=[C:42]([F:46])[C:41]=1[CH2:47][CH2:48][NH:49][C:50]1[CH:55]=[C:54]([C:56]2[CH:61]=[CH:60][CH:59]=[C:58]([O:62][CH3:63])[CH:57]=2)[N:53]=[C:52]([O:64][CH3:65])[N:51]=1.Cl>CCO.CCOCC.C(#N)C>[ClH:1].[Cl:39][C:40]1[CH:45]=[CH:44][CH:43]=[C:42]([F:46])[C:41]=1[CH2:47][CH2:48][NH:49][C:50]1[CH:55]=[C:54]([C:56]2[CH:61]=[CH:60][CH:59]=[C:58]([O:62][CH3:63])[CH:57]=2)[N:53]=[C:52]([O:64][CH3:65])[N:51]=1

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 951534-NitrophenethylamineHCID 11494834HCID 11494834、化合物HCID 57636022[2-(2-Chloro-6-fluoro-phenyl)-ethyl]-[2-methoxy-6-(3-methoxy-phenyl)-pyrimidin-4-yl]-amine

生成物 1

HCID 69073584HCID 69073584、化合物収率 60%

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 3283Diethyl Ether溶媒2 回HCID 6342Acetonitrile溶媒

実験手順

By proceeding in a similar manner to Example 43(b) but (i) substituting 2-(2-chloro-6-fluoro-phenyl)-ethylamine for 2-(4-nitro-phenyl)-ethylamine, acetonitrile for EtOH as solvent in Step 3 there is prepared [2-(2-chloro-6-fluoro-phenyl)-ethyl]-[2-methoxy-6-(3-methoxy-phenyl)-pyrimidin-4-yl]-amine which is dissolved in ether and treated with 1 M hydrogen chloride in ether to afford [2-(2-chloro-6-fluoro-phenyl)-ethyl]-[2-methoxy-6-(3-methoxy-phenyl)-pyrimidin-4-yl]-amine hydrochloride [51 mg, 60%, Example 43(d)] as a solid. LC/MS: RT=2.82 minutes MS: 388 (M+H). 1H NMR [300 MHz, (CD3)2SO]: □7.12-7.48 (7H, m), 6.6 (1H, s), 3.99 (3H, s), 3.82 (3H, s), 3.67 (2H, m), 3.07 (2H, m).

出典と根拠

ORDレコード
ord-d6b9edde907644119e3a00e6b2e073cb
出典データセット
uspto-grants-2012_06
特許番号
US08193183B2

関連ノート

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