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Cyclohexane → HCID 54227761, 화합물

HRID 1658022
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HRID 1658022 반응식
C(=[N:8][CH:9]([P:23]([O:32][C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1)([O:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)=[O:24])[C:10]([O:12][CH2:13][C:14]1[CH:19]=[CH:18][C:17]([N+:20]([O-:22])=[O:21])=[CH:16][CH:15]=1)=[O:11])C1C=CC=CC=1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1.C1CCCCC1>C(OCC)C>[NH2:8][CH:9]([P:23]([O:25][C:26]1[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1)([O:32][C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1)=[O:24])[C:10]([O:12][CH2:13][C:14]1[CH:19]=[CH:18][C:17]([N+:20]([O-:22])=[O:21])=[CH:16][CH:15]=1)=[O:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8078CyclohexaneHCID 521998p-Toluenesulfonic acid monohydrateHCID 54211819HCID 54211819, 화합물

생성물 1

HCID 54227761HCID 54227761, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

A solution of p-nitrobenzyl N-benzylidene-α-aminodiphenylphosphonoacetate (16.43 g) in ethyl ether (100 ml) is added dropwise over 30 minutes to a stirring solution of p-toluenesulfonic acid monohydrate (6.48 g) in ethyl ether (150 ml). Cyclohexane (100 ml) is added to the mixture and the solvents are decanted from the precipitate. The precipitate is washed with more 2:1 ethyl ether-cyclohexane which is again decanted off. The precipitate is treated with 1 M aqueous dipotassium hydrogen phosphate (60 ml) and extracted with four portions of methylene chloride. The methylene chloride solution is dried over magnesium sulfate, filtered, and evaporated to give p-nitrobenzyl α-aminodiphenylphosphonacetate.

후처리

  1. customthe solvents are decanted from the precipitate
  2. washThe precipitate is washed with more 2:1 ethyl ether-cyclohexane which
  3. customis again decanted off
  4. additionThe precipitate is treated with 1 M aqueous dipotassium hydrogen phosphate (60 ml)
  5. extractionextracted with four portions of methylene chloride
  6. dry with materialThe methylene chloride solution is dried over magnesium sulfate
  7. filtrationfiltered
  8. customevaporated
  9. customto give p-nitrobenzyl α-aminodiphenylphosphonacetate

출처 및 근거

ORD 기록
ord-6722a63cf2ac4628b79726730a1a5ee2
출처 데이터셋
uspto-grants-1976_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03962224

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