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Dichloromethane → HCID 15052137, 화합물

HRID 973435
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HRID 973435 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8][CH2:9][CH:10]([C:14]1[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[C:16]([O:22][CH3:23])[CH:15]=1)[C:11](O)=[O:12].C(Cl)Cl.Cl.C(N=C=NCCCN(C)C)C>C(N(CC)CC)C>[CH3:23][O:22][C:16]1[CH:15]=[C:14]([CH:10]2[C:11](=[O:12])[NH:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=3[S:8][CH2:9]2)[CH:19]=[CH:18][C:17]=1[O:20][CH3:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 15052136HCID 15052136, 화합물

생성물 1

HCID 15052137HCID 15052137, 화합물수율 90.6%

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

A solution of 9.1 g of the product of Step C, 180 ml of methylene chloride, 6.25 g of 1-ethyl-3-(3-dimethylamino propyl) carbodiimide hydrochloride and 9 ml of triethylamine was stirred for 90 minutes at ambient temperature and the methylene chloride was evaporated off. The residue was taken up in 90 ml of ethyl acetate and after separation, 7.8 g of the expected product were obtained melting at 174° C. An analytical sample was obtained by crystallization of 200 mg of crude product from 10 ml of ethyl acetate to obtain 120 mg of the desired product melting at 184° C.

후처리

  1. customthe methylene chloride was evaporated off
  2. customafter separation

출처 및 근거

ORD 기록
ord-db3fef344be9476fae908882e09a5a74
출처 데이터셋
uspto-grants-1991_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05063225

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