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Sodium Carbonate → N1,N1-Dibenzylethane-1,2-diamine

HRID 1287322
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HRID 1287322 반응식
C(=O)([O-])[O-].[Na+].[Na+].C(OC(N1C(=O)C2=CC=CC=C2C1=O)=O)C.C(O)(=O)C.[CH2:27]([N:34]([CH2:38][C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1)[CH2:35][CH2:36][NH2:37])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.CC12CC1(C(O)=O)N1C(=O)C(N3C(=O)C4=CC=CC=C4C3=O)[C@H]1S2>CC12CC1(C(O)=O)N1C(=O)C(N)[C@H]1S2.O.CO>[CH2:38]([N:34]([CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)[CH2:35][CH2:36][NH2:37])[C:39]1[CH:40]=[CH:41][CH:42]=[CH:43][CH:44]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 10340Sodium CarbonateHCID 31187N-CarbethoxyphthalimideHCID 19828334N,N-dibenzylethylenediamine acetateHCID 681326432-Methyl-2,3-methylene-6-phthalimidopenam-3-carboxylic acid

생성물 1

HCID 6394114N1,N1-Dibenzylethane-1,2-diamine수율 159.1%

시약·촉매·용매 3

HCID 887
Methanol
용매
HCID 962Water용매2회
HCID 681320312-Methyl-2,3-methylene-6-aminopenam-3-carboxylic acid용매

실험 절차

Sodium carbonate (212 mg.) was dissolved in a suspension of 2-methyl-2,3-methylene-6-aminopenam-3-carboxylic acid (428 mg.) in water (4 ml.). To a solution was added N-ethoxycarbonylphthalimide (440 mg.) all at once, and then stirred at room temprature for 2 hours. The resultant mixture was washed with methylene chloride. Methylene chloride (20 ml.) was added to the mixture, and then the solution was acidified with 1/4N-hydrochloric acid (16 ml.) and extracted. The extract was washed with water, dried over magnesium sulfate and then the solvent removed under reduced pressure to give amorphous product. The product was dissolved in methanol (8 ml.). To the solution was added an aqueous solution of N,N-dibenzylethylenediamine acetate (220 mg.) in water (4 ml.) to give colorless crystals of N,N-dibenzylethylenediamine salt (280 mg.) of 2-methyl-2,3-methylene-6-phthalimidopenam-3-carboxylic acid, mp 181° to 182°C (dec.).

후처리

  1. washThe resultant mixture was washed with methylene chloride
  2. additionMethylene chloride (20 ml.) was added to the mixture
  3. extractionextracted
  4. washThe extract was washed with water
  5. dry with materialdried over magnesium sulfate
  6. customthe solvent removed under reduced pressure
  7. customto give amorphous product

출처 및 근거

ORD 기록
ord-76e8ab8e8802456e9f11c6b6f1af73d6
출처 데이터셋
uspto-grants-1976_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03984397

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