Diisopropylethylamine → HCID 178479421, 화합물

HRID 619268노트

반응식

HRID 619268 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 178479421HCID 178479421, 화합물수율 112.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-48ab38778dca470eac8a95b03650cb42
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05958944

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