Triethylamine → HCID 45274965、化合物

HRID 1942898ノート

反応式

HRID 1942898 の反応式
Cl.[NH:2]1[CH2:7][CH2:6][CH:5]([CH2:8][C:9]([OH:11])=[O:10])[CH2:4][CH2:3]1.C(N(CC)CC)C.Cl[C:20]1[N:25]=[C:24]([O:26][CH3:27])[N:23]=[C:22]([NH:28][C:29]2[CH:34]=[CH:33][C:32]([N:35]3[CH:39]=[C:38]([CH3:40])[N:37]=[CH:36]3)=[C:31]([O:41][CH3:42])[CH:30]=2)[N:21]=1>CO>[CH3:27][O:26][C:24]1[N:23]=[C:22]([NH:28][C:29]2[CH:34]=[CH:33][C:32]([N:35]3[CH:39]=[C:38]([CH3:40])[N:37]=[CH:36]3)=[C:31]([O:41][CH3:42])[CH:30]=2)[N:21]=[C:20]([N:2]2[CH2:7][CH2:6][CH:5]([CH2:8][C:9]([OH:11])=[O:10])[CH2:4][CH2:3]2)[N:25]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 155657754-Piperidineacetic acid hydrochlorideHCID 86640783(4-Chloro-6-methoxy-[1,3,5]triazin-2-yl)-[3-methoxy-4-(4-methyl-imidazol-1-yl)-phenyl]-amine

生成物 1

HCID 45274965HCID 45274965、化合物収率 87%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

4-Piperidineacetic acid hydrochloride (381 mg, 2.12 mmol) was suspended in 10 ml of methanol. Triethylamine (0.9 ml, 6.45 mmol) was added, followed by (4-chloro-6-methoxy-[1,3,5]triazin-2-yl)-[3-methoxy-4-(4-methyl-imidazol-1-yl)-phenyl]-amine (700 mg, 2.02 mmol). The resulting mixture was stirred overnight at room temperature, concentrated and subjected to column chromatography on Si—NH2 (Isolute) using dichloromethane/methanol 95:5 v/v as an eluent. The material isolated was further purified by several triturations in water to give the final compound (792 mg, 87%) as a slightly brownish solid.

後処理

  1. concentrationconcentrated
  2. customThe material isolated
  3. customwas further purified by several triturations in water

出典と根拠

ORDレコード
ord-004c6de6cecd4cfa813dbc55dce7cf40
出典データセット
uspto-grants-2013_03
特許番号
US08389717B2

反応ノート

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