Sodium Bicarbonate → 2-{4-[2-Amino-6-({[2-(4-chlorophenyl)-1,3-thiazol-4-yl]methyl}thio)-3,5-dicyanopyridin-4-yl]-piperidin-1-yl}-2-oxoethyl acetate

HRID 1873574ノート

反応式

HRID 1873574 の反応式
[C:1]([O:4][CH2:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]2[C:19]([C:20]#[N:21])=[C:18]([SH:22])[N:17]=[C:16]([NH2:23])[C:15]=2[C:24]#[N:25])[CH2:10][CH2:9]1)=[O:7])(=[O:3])[CH3:2].Cl[CH2:27][C:28]1[N:29]=[C:30]([C:33]2[CH:38]=[CH:37][C:36]([Cl:39])=[CH:35][CH:34]=2)[S:31][CH:32]=1.C(=O)(O)[O-].[Na+]>CN(C=O)C>[C:1]([O:4][CH2:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]2[C:19]([C:20]#[N:21])=[C:18]([S:22][CH2:27][C:28]3[N:29]=[C:30]([C:33]4[CH:38]=[CH:37][C:36]([Cl:39])=[CH:35][CH:34]=4)[S:31][CH:32]=3)[N:17]=[C:16]([NH2:23])[C:15]=2[C:24]#[N:25])[CH2:10][CH2:9]1)=[O:7])(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 6102974-(Chloromethyl)-2-(4-chlorophenyl)-1,3-thiazoleHCID 178476478HCID 178476478、化合物

生成物 1

HCID 687021312-{4-[2-Amino-6-({[2-(4-chlorophenyl)-1,3-thiazol-4-yl]methyl}thio)-3,5-dicyanopyridin-4-yl]-piperidin-1-yl}-2-oxoethyl acetate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

34 mg (0.06 mmol) of the compound from Example 24A are dissolved in 1.2 ml of dry DMF, and 17 mg (0.07 mmol) of 4-(chloromethyl)-2-(4-chlorophenyl)-1,3-thiazole and 19 mg (0.23 mmol) of sodium bicarbonate are added. The reaction mixture is stirred at RT for 8 h. The mixture is then filtered, and about 0.5 ml of water is added to the filtrate. The precipitate formed is filtered off with suction and dried under reduced pressure at +50° C.

後処理

  1. filtrationThe mixture is then filtered
  2. additionabout 0.5 ml of water is added to the filtrate
  3. customThe precipitate formed
  4. filtrationis filtered off with suction
  5. customdried under reduced pressure at +50° C.

出典と根拠

ORDレコード
ord-808f51f1d05b4497b1c1c2c855bd4334
出典データセット
uspto-grants-2012_11
特許番号
US08304412B2

反応ノート

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