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HCID 12804816、化合物 → HCID 12805476、化合物

HRID 258426
ノート
印刷プレビュー

反応式

HRID 258426 の反応式
S1C2C=CC=CC=2N=C1S[S:11][C@H:12]1[N:15]([CH:16]([C:33]([CH3:35])=[CH2:34])[C:17]([O:19][CH:20]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[O:18])[C:14](=[O:36])[C@H:13]1[NH:37][C:38](=[O:47])[CH2:39][O:40][C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1.O.[C:49]1([CH3:58])[CH:54]=[CH:53][C:52]([S:55]([O-:57])=[O:56])=[CH:51][CH:50]=1.[Na+]>CC(C)=O.O.[N+]([O-])([O-])=O.[Ag+]>[C:49]1([CH3:58])[CH:54]=[CH:53][C:52]([S:55]([S:11][C@H:12]2[N:15]([CH:16]([C:33]([CH3:35])=[CH2:34])[C:17]([O:19][CH:20]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=3)=[O:18])[C:14](=[O:36])[C@H:13]2[NH:37][C:38](=[O:47])[CH2:39][O:40][C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)(=[O:57])=[O:56])=[CH:51][CH:50]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 12804816HCID 12804816、化合物HCID 23682957Sodium 4-methylbenzene-1-sulfinate hydrate

生成物 1

HCID 12805476HCID 12805476、化合物収率 74.1%

試薬・触媒・溶媒 3

HCID 24470Silver Nitrate触媒HCID 180Acetone溶媒3 回
HCID 962
Water
溶媒
2 回

実験手順

To a solution of diphenylmethyl 2-[(3R,4R)-4-[(benzothiazol-2-yl)dithio]-3-phenoxyacetamido-2-oxo-azetidin-1-yl]-3-methyl-3-butenoate (XIIIa. 12.12 g, 0.0182 mole) in acetone (325 mL) and water (37 mL), silver nitrate (3.86 g, 0.0227 mole) was added all at once. A freshly prepared solution of sodium p-toluenesulfinate hydrate (4.05 g; 0.0227 mole) in acetone (255 mL) and water (37 mL) was added dropwise over 1 h, while the reaction mixture was protected from light. After an additional 1h period at room temperature, Celite (5 g) was added and the mixture was diluted with acetone (500 mL) and then was filtered. The filtrate was evaporated to a small volume, and the crude product was extracted into ether (3×250 mL). The ether phase was dried with magnesium sulfate and concentrated to afford a crude product. Flash chromatography (SiO2, eluting with 40% ethyl acetate in hexane) gave 9.05 g (73.5%) of the title compound as a white solid.

後処理

  1. filtrationwas filtered
  2. customThe filtrate was evaporated to a small volume
  3. extractionthe crude product was extracted into ether (3×250 mL)
  4. dry with materialThe ether phase was dried with magnesium sulfate
  5. concentrationconcentrated
  6. customto afford a crude product
  7. washFlash chromatography (SiO2, eluting with 40% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-8d4c6a772b084f35beba24f23dfdd98d
出典データセット
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05266691

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート