Dichloromethane → N,N'-Bis(1-methylethyl)urea

HRID 1680016

반응식

HRID 1680016 반응식
C(C1(C(NC(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)C(O)=O)NC(C(OCC2C=CC=CC=2)=[O:14])C2(CCNCC2)S1)C1C=CC=CC=1.[CH:52]([N:55]=[C:56]=[N:57][CH:58]([CH3:60])[CH3:59])([CH3:54])[CH3:53].ClCCl.[N+](C)([O-])=O>C(Cl)(Cl)Cl>[CH:52]([NH:55][C:56]([NH:57][CH:58]([CH3:60])[CH3:59])=[O:14])([CH3:54])[CH3:53]

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 6375NitromethaneHCID 12734DiisopropylcarbodiimideHCID 54040992Benzyl-4-benzyloxycarbonyl-alpha-tritylamino-1-thia-3,8-diazaspiro[4.5]decane-2-acetic acid

생성물 1

HCID 20084N,N'-Bis(1-methylethyl)urea

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

The reation between 8 benzyl-4-benzyloxycarbonyl-alpha- tritylamino-1-thia-3,8-diazaspiro[4.5 ]decane-2-acetic acid (obtained in 6.2.) and diisopropylcarbodiimide (80 g) can be performed in chloroform (400 ml), dichloromethane or a mixture of nitromethane and chloroform, either at ambient temperature, leaving the mixture to stand for 4 weeks, or at 50° C. for 12 hours. In all cases, the 1,3-diisopropylurea formed is removed by filtration, the solvent and excess reagent are evaporated and the residue is passed through a column of silica gel (60 Merck), using chloroform as eluent. In all cases, benzyl 1°-benzyl-6-tritylamino-spiro[penam-2,4'-piperidine ]-3-carboxylate is obtained, which is crystallized from diethy ether in a yield of 25 to 40%; M.P. 191°-192° C. (recrystallized from acetonitrile).

후처리

  1. customat ambient temperature, leaving the mixture
  2. waitto stand for 4 weeks

출처 및 근거

ORD 기록
ord-4a7ed9f736984c9e90370b28b011d553
출처 데이터셋
uspto-grants-1981_06
특허 번호
US04271172

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