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2-(Dimethylamino)acetyl chloride hydrochloride → 1-(3-Methoxycarbonyl-2-thioureido)-2-(2-dimethylaminoacetamido)-4-thiocyanatobenzene hydrochloride

HRID 258765
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인쇄 미리보기

반응식

HRID 258765 반응식
[NH2:1][C:2]1[CH:7]=[C:6]([S:8][C:9]#[N:10])[CH:5]=[CH:4][C:3]=1[NH:11][C:12]([NH:14][C:15]([O:17][CH3:18])=[O:16])=[S:13].Cl.[CH3:20][N:21]([CH3:26])[CH2:22][C:23]([Cl:25])=[O:24]>ClCCl>[ClH:25].[CH3:18][O:17][C:15]([NH:14][C:12](=[S:13])[NH:11][C:3]1[CH:4]=[CH:5][C:6]([S:8][C:9]#[N:10])=[CH:7][C:2]=1[NH:1][C:23](=[O:24])[CH2:22][N:21]([CH3:26])[CH3:20])=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 139949912-(Dimethylamino)acetyl chloride hydrochlorideHCID 214266632-Amino-1-(3-methoxycarbonyl-2-thioureido)-4-thiocyanatobenzene

생성물 1

HCID 214266061-(3-Methoxycarbonyl-2-thioureido)-2-(2-dimethylaminoacetamido)-4-thiocyanatobenzene hydrochloride수율 54.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A stirred suspension of 2-amino-1-(3-methoxycarbonyl-2-thioureido)-4-thiocyanatobenzene (5.6 g.) in dichloromethane (190 ml.) was treated in one portion at room temperature with N,N-dimethylglycyl chloride hydrochloride (3.82 g.). The stirring was continued for one hour and the mixture was allowed to stand overnight. The solid was filtered off and recrystallised from methanol to give 1-(3-methoxycarbonyl-2-thioureido)-2-(2-dimethylaminoacetamido)-4-thiocyanatobenzene hydrochloride (4.35 g.), m.p. 192°-193° C. (with decomposition).

후처리

  1. waitto stand overnight
  2. filtrationThe solid was filtered off
  3. customrecrystallised from methanol

출처 및 근거

ORD 기록
ord-48c2ac14960a4e8f80d31f2502127527
출처 데이터셋
uspto-grants-1977_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04034107

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