Ethyl Acetate → HCID 178452375, 화합물

HRID 2289054노트

반응식

HRID 2289054 반응식
[N+:1]([C:4]1[CH:34]=[CH:33][C:7]([CH2:8][O:9][C:10]([N:12]=[C:13]([NH:19][C:20](=[O:32])[O:21][CH2:22][C:23]2[CH:28]=[CH:27][C:26]([N+:29]([O-:31])=[O:30])=[CH:25][CH:24]=2)N2C=CC=N2)=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2].[NH2:35][CH2:36][C:37]([NH:39][CH:40]1[CH2:43][N:42]([C:44]([O:46][C:47]([CH3:50])([CH3:49])[CH3:48])=[O:45])[CH2:41]1)=[O:38].C(OCC)(=O)C>O1CCCC1>[N+:1]([C:4]1[CH:5]=[CH:6][C:7]([CH2:8][O:9][C:10]([N:12]=[C:13]([NH:19][C:20]([O:21][CH2:22][C:23]2[CH:28]=[CH:27][C:26]([N+:29]([O-:31])=[O:30])=[CH:25][CH:24]=2)=[O:32])[NH:35][CH2:36][C:37]([NH:39][CH:40]2[CH2:43][N:42]([C:44]([O:46][C:47]([CH3:50])([CH3:49])[CH3:48])=[O:45])[CH2:41]2)=[O:38])=[O:11])=[CH:33][CH:34]=1)([O-:3])=[O:2]

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 18699815Tert-butyl 3-(2-aminoacetamido)azetidine-1-carboxylateHCID 54574361HCID 54574361, 화합물

생성물 1

HCID 178452375HCID 178452375, 화합물수율 101.6%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Under ice cooling, a solution of 4-nitrobenzyl [(4-nitrobenzyloxy)carbonyliminopyrazol-1-ylmethyl]carbamate (1.42 g) in tetrahydrofuran (12 ml) was added to a solution of tert-butyl 3-(aminoacetylamino)-1-azetidinecarboxylate (785 mg) in tetrahydrofuran (13 ml) and the mixture was stirred at room temperature for 3 hours. Ethyl acetate was added to the reaction mixture. The resulting mixture was washed with water, an aqueous solution of potassium hydrogensulfate and saturated saline, dried over anhydrous magnesium sulfate and concentrated by evaporation under reduced pressure. The residue was crystallized from diisopropyl ether, followed by washing, whereby 1.94 g of the title compound were obtained as a colorless crystals.

후처리

  1. washThe resulting mixture was washed with water
  2. dry with materialan aqueous solution of potassium hydrogensulfate and saturated saline, dried over anhydrous magnesium sulfate
  3. concentrationconcentrated by evaporation under reduced pressure
  4. customThe residue was crystallized from diisopropyl ether
  5. washby washing

출처 및 근거

ORD 기록
ord-1e55bd4abc8d44cc8cb873cd09d7b743
출처 데이터셋
uspto-grants-2000_07
특허 번호
US06090802

반응 노트

불러오는 중…