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Acetic Acid → HCID 178476691, 화합물

HRID 479569
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HRID 479569 반응식
[C:1]([OH:4])(=[O:3])[CH3:2].[Cl:5][C:6]1[C:15]2[C:10](=[CH:11][C:12]([C:16]3[CH:21]=[CH:20][CH:19]=[C:18]([C:22]#[N:23])[CH:17]=3)=[CH:13][CH:14]=2)[C:9]([NH:24][C:25]([NH2:27])=[NH:26])=[N:8][CH:7]=1>COCCOC.CN1C(=O)CCC1>[C:1]([O-:4])(=[O:3])[CH3:2].[Cl:5][C:6]1[C:15]2[C:10](=[CH:11][C:12]([C:16]3[CH:21]=[CH:20][CH:19]=[C:18]([C:22]#[N:23])[CH:17]=3)=[CH:13][CH:14]=2)[C:9]([NH:24][C:25]([NH2:27])=[NH2+:26])=[N:8][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 176Acetic AcidHCID 178509681HCID 178509681, 화합물

생성물 1

HCID 178476691HCID 178476691, 화합물수율 143%

시약·촉매·용매 2

HCID 80711,2-Dimethoxyethane용매HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

A solution of acetic acid (0.72 kg, mol) in DME (13.6 L) was added dropwise to a stirred solution of (4-chloro-7-(3-cyanophenyl)isoquinolin-1-yl)guanidine (4.4 kg, 13.7 mol) in NMP (14 kg) at 100° C. After addition the thick slurry was allowed to cool and was stirred overnight at room temperature. The solid was collected by filtration, washed with DME (4.9 L) and dried overnight in vacuo at 50° C. to give (4-chloro-7-(3-cyanophenyl)isoquinolin-1-yl)guanidinium acetate (6 kg, 143%) as an NMP wet off white solid.

후처리

  1. additionAfter addition the thick slurry
  2. temperatureto cool
  3. filtrationThe solid was collected by filtration
  4. washwashed with DME (4.9 L)
  5. customdried overnight in vacuo at 50° C.

출처 및 근거

ORD 기록
ord-ae65cef656d145368ff3a02a1bf37d59
출처 데이터셋
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06645979B2

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