Triethylamine → Revaprazan Hydrochloride

HRID 1069412ノート

反応式

HRID 1069412 の反応式
C(N(CC)CC)C.CC1C2C(=CC=CC=2)CCN1.[Cl:19]C1C(C)=C(C)N=C(NC2C=CC(F)=CC=2)N=1.[CH3:36][C:37]1[C:38]([N:52]2[CH2:61][CH2:60][C:59]3[C:54](=[CH:55][CH:56]=[CH:57][CH:58]=3)[CH:53]2[CH3:62])=[N:39][C:40]([NH:44][C:45]2[CH:50]=[CH:49][C:48]([F:51])=[CH:47][CH:46]=2)=[N:41][C:42]=1[CH3:43]>C(O)CO.C(O)CCC>[ClH:19].[CH3:36][C:37]1[C:38]([N:52]2[CH2:61][CH2:60][C:59]3[C:54](=[CH:55][CH:56]=[CH:57][CH:58]=3)[CH:53]2[CH3:62])=[N:39][C:40]([NH:44][C:45]2[CH:50]=[CH:49][C:48]([F:51])=[CH:47][CH:46]=2)=[N:41][C:42]=1[CH3:43]

参加物

7

反応物 4

HCID 8471TriethylamineHCID 922141-Methyl-1,2,3,4-tetrahydroisoquinolineHCID 204104RevaprazanHCID 99923764-Chloro-N-(4-fluorophenyl)-5,6-dimethylpyrimidin-2-amine

生成物 1

HCID 204103Revaprazan Hydrochloride収率 91%

試薬・触媒・溶媒 2

HCID 174Ethylene Glycol溶媒HCID 2631-Butanol溶媒

実験手順

8.12 g (11.2 ml, 80.3 mmole) of triethylamine, 30 ml of n-butanol and 6.58 g (44.1 mmole) of 1-methyl-1,2,3,4-tetrahydroisoquinoline were added to 40 ml of ethylene glycol. 10.1 g (40.1 mmole) of 4-chloro-2-(4-fluorophenylamino)-5,6-dimethylpyrimidine was added thereto and then reacted at 130° C. for 30 hours under refluxing to prepare 5,6-dimethyl-2-(4-fluorophenylamino)-4-(1-methyl-1,2,3,4-tetrahydroisoquinolin-2-yl)-pyrimidine. This product was treated according to the procedure detailed in Example 14 to obtain 14.7 g of purified 5,6-dimethyl-2-(4-fluorophenylamino)-4-(1-methyl-1,2,3,4-tetrahydroisoquinolin-2-yl)pyrimidine hydrochloride.

後処理

  1. customreacted at 130° C. for 30 hours
  2. temperatureunder refluxing
  3. additionThis product was treated

出典と根拠

ORDレコード
ord-8a7361587a5348938c175c46cfc4ce87
出典データセット
uspto-grants-2001_06
特許番号
US06252076B1

反応ノート

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