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Trisodium;borate;decahydrate → 3-Amino-3-methoxy-2-oxo-1-azetidinesulfonic acid tetrabutylammonium salt

HRID 867633
ノート
印刷プレビュー

反応式

HRID 867633 の反応式
O.O.O.O.O.O.O.O.O.O.B([O-])([O-])[O-].[Na+].[Na+].[Na+].[CH2:18]([N+:22]([CH2:31][CH2:32][CH2:33][CH3:34])([CH2:27][CH2:28][CH2:29][CH3:30])[CH2:23][CH2:24][CH2:25][CH3:26])[CH2:19][CH2:20][CH3:21].[CH3:35][O:36][C:37]1([NH:46]C(OCC2C=CC=CC=2)=O)[CH2:40][N:39]([S:41]([O-:44])(=[O:43])=[O:42])[C:38]1=[O:45]>CO.[Pd]>[CH2:31]([N+:22]([CH2:18][CH2:19][CH2:20][CH3:21])([CH2:23][CH2:24][CH2:25][CH3:26])[CH2:27][CH2:28][CH2:29][CH3:30])[CH2:32][CH2:33][CH3:34].[NH2:46][C:37]1([O:36][CH3:35])[CH2:40][N:39]([S:41]([O-:44])(=[O:42])=[O:43])[C:38]1=[O:45]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 18377803Trisodium;borate;decahydrateHCID 1317142663-Methoxy-2-oxo-3-[[(phenylmethoxy)carbonyl]amino]-1-azetidinesulfonic acid, tetrabutylammonium salt

生成物 1

HCID 1317142653-Amino-3-methoxy-2-oxo-1-azetidinesulfonic acid tetrabutylammonium salt収率 76.2%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887
Methanol
溶媒
3 回

実験手順

A 4% sodium borate decahydrate in methanol solution (100 μl) is added to a suspension of 10% palladium on charcoal (30 mg) in methanol (2 ml), and the mixture is stirred under an atmosphere of hydrogen for 15 minutes. 3-Methoxy-2-oxo-3-[[(phenylmethoxy)carbonyl]amino]-1-azetidinesulfonic acid, tetrabutylammonium salt (60 mg; see Example 49) in methanol (2 ml) is added and the mixture is vigorously stirred for 15 minutes under a hydrogen atmosphere. Catalyst is removed by filtration through Celite on a millipore filter (0.5 mμ), and solvent is removed from the filtrate in vacuo, and the residue is extracted with methylene chloride. Removal of solvent under reduced pressure yields 35 mg of the title compound, as an oil.

後処理

  1. stirringthe mixture is vigorously stirred for 15 minutes under a hydrogen atmosphere
  2. customCatalyst is removed by filtration through Celite on a millipore
  3. filtrationfilter (0.5 mμ), and solvent
  4. customis removed from the filtrate in vacuo
  5. extractionthe residue is extracted with methylene chloride
  6. customRemoval of solvent under reduced pressure

出典と根拠

ORDレコード
ord-912e3efdf95c4222b59447ed65508ac9
出典データセット
uspto-grants-1988_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04775670

反応ノート

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