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Hydrochloric Acid → HCID 57819764、化合物

HRID 2380828
ノート
印刷プレビュー

反応式

HRID 2380828 の反応式
Cl[C:2]1[N:7]=[C:6]([N:8]2[CH2:13][CH2:12][C:11]3[N:14]=[CH:15][NH:16][C:10]=3[CH2:9]2)[C:5]([N:17]([CH3:19])[CH3:18])=[CH:4][N:3]=1.O.Cl.[CH3:22][N:23]([CH2:25][C:26]1[CH:31]=[CH:30][C:29]([NH2:32])=[CH:28][CH:27]=1)[CH3:24]>O1CCOCC1.CN(C=O)C>[CH3:24][N:23]([CH2:25][C:26]1[CH:27]=[CH:28][C:29]([NH:32][C:2]2[N:7]=[C:6]([N:8]3[CH2:13][CH2:12][C:11]4[N:14]=[CH:15][NH:16][C:10]=4[CH2:9]3)[C:5]([N:17]([CH3:19])[CH3:18])=[CH:4][N:3]=2)=[CH:30][CH:31]=1)[CH3:22]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 308051Benzenemethanamine, 4-amino-N,N-dimethyl-HCID 21081013HCID 21081013、化合物

生成物 1

HCID 57819764HCID 57819764、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒
HCID 31275
1,4-Dioxane
溶媒

反応条件

温度
95 °C

実験手順

50 mg 2-chloro-4-(3,4,6,7-tetrahydro-imidazo[4,5-c]pyridin-5-yl)-5-dimethylamino-pyrimidine are suspended in 60 μL of 1,4-dioxane, 20 μL water and 90 μL of a 5 M hydrochloric acid (in 1,4-dioxane) and mixed with 55 mg 4-dimethylaminomethyl-phenylamine. This mixture is heated to 95° C. and stirred for 20 h at this temperature. The suspension obtained is diluted with DMF and then purified by column chromatography. The carrier material used is C18-RP-silica gel and a gradient is run through which consists at the starting point of 95% water (10 mM ammonium hydrogen carbonate and 38 mM ammonia) and 5% acetonitrile and at the finishing point of 50% water and 50% acetonitrile. The fractions are freeze-dried. The residue is taken up in acetonitrile, combined with aqueous hydrochloric acid and freeze-dried once more.

後処理

  1. customThe suspension obtained
  2. custompurified by column chromatography
  3. customThe fractions are freeze-dried
  4. customfreeze-dried once more

出典と根拠

ORDレコード
ord-de4459fe418c4107ab0138afcc27f787
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08258129B2

反応ノート

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