Ethyl Acetate → HCID 178452375、化合物

HRID 2289054ノート

反応式

HRID 2289054 の反応式
[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]

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 18699815Tert-butyl 3-(2-aminoacetamido)azetidine-1-carboxylateHCID 54574361HCID 54574361、化合物

生成物 1

HCID 178452375HCID 178452375、化合物収率 101.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1e55bd4abc8d44cc8cb873cd09d7b743
出典データセット
uspto-grants-2000_07
特許番号
US06090802

反応ノート

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