Diisopropylethylamine → HCID 178479421、化合物

HRID 619268ノート

反応式

HRID 619268 の反応式
[ClH:1].[N:2]1([C:7]([NH2:9])=[NH:8])[CH:6]=[CH:5][CH:4]=N1.Cl.Cl.[N:12]1[CH:17]=[CH:16][C:15]([NH:18][C:19](=[O:28])[C:20]2[CH:25]=CC(CN)=[CH:22][CH:21]=2)=[CH:14][CH:13]=1.C(N(C(C)C)CC)(C)C>CO>[OH2:28].[ClH:1].[N:12]1[CH:17]=[CH:16][C:15]([NH:18][C:19](=[O:28])[C:20]2[CH:21]=[CH:22][C:5]([CH2:6][NH:2][C:7]([NH2:9])=[NH:8])=[CH:4][CH:25]=2)=[CH:14][CH:13]=1

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 2734672Pyrazole-1-carboxamidine monohydrochlorideHCID 221206014-(aminomethyl)-N-(pyridin-4-yl)benzamide dihydrochloride

生成物 1

HCID 178479421HCID 178479421、化合物収率 112.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Pyrazole-1-carboxamidine hydrochloride (540 mg) was added to a solution of N-(4-pyridyl)-4-aminomethylbenzamide dihydrochloride (550 mg) and diisopropylethylamine (950 mg) in methanol (7 ml), and the mixture was stirred in a stream of nitrogen at room temperature for 6 hours. After the reaction, the reaction mixture was concentrated to half under reduced pressure, and ethyl acetate was added to precipitate crystals. The crystals were collected by filtration, and recrystallized from methanol-ethyl acetate to give 333 mg of N-(4-pyridyl)-4-guanidinomethylbenzamide monohydrochloride monohydrate having a melting point of 244-248° C.

後処理

  1. customAfter the reaction
  2. concentrationthe reaction mixture was concentrated to half under reduced pressure, and ethyl acetate
  3. additionwas added
  4. customto precipitate crystals
  5. filtrationThe crystals were collected by filtration
  6. customrecrystallized from methanol-ethyl acetate

出典と根拠

ORDレコード
ord-48ab38778dca470eac8a95b03650cb42
出典データセット
uspto-grants-1999_09
特許番号
US05958944

反応ノート

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