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Sodium Azide → HCID 14555476, 화합물

HRID 232043
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HRID 232043 반응식
CS(O[C@@H:6]1[CH2:10][CH2:9][N:8]([C:11]([O:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[O:12])[CH2:7]1)(=O)=O.[N-:21]=[N+:22]=[N-:23].[Na+]>CN(C)C=O>[N:21]([C@H:6]1[CH2:10][CH2:9][N:8]([C:11]([O:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[O:12])[CH2:7]1)=[N+:22]=[N-:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 33557Sodium AzideHCID 14555473(R)-1-((Benzyloxy)carbonyl)pyrrolidin-3-yl methanesulfonate

생성물 1

HCID 14555476HCID 14555476, 화합물수율 91.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 20.5 g (72 mmol) of (R)-3-[(methylsulfonyl)oxy]-1-pyrrolidinecarboxylic acid, phenylmethyl ester in 100 ml of dry N,N-dimethylformamide was treated with 6.5 g (0.1 mol) of sodium azide and heated at 90° for four hours. The solvent was removed in high vacuo at 50° and the residue was partitioned between ethyl acetate/water (250 ml each). The aqueous layer was reextracted with ethyl acetate and the combined organic fractions were washed with water, dried (MgSO4) and evaporated in vacuo to give 16.2 g of the title compound.

후처리

  1. temperatureheated at 90° for four hours
  2. customThe solvent was removed in high vacuo at 50°
  3. customthe residue was partitioned between ethyl acetate/water (250 ml each)
  4. washthe combined organic fractions were washed with water
  5. dry with materialdried (MgSO4)
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-a1255020776e4556adb0c1e2e04b21f7
출처 데이터셋
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04851418

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