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Boron trifluoride etherate → HCID 13422884、化合物

HRID 2290419
ノート
印刷プレビュー

反応式

HRID 2290419 の反応式
B(F)(F)F.CCOCC.[C:10]1([C:16]2[O:22][C@H:21]3[C@H:18]([C:19](=[O:23])[NH:20]3)[N:17]=2)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.[OH:24][CH2:25][C:26](=[O:35])[CH2:27][C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29].C([O-])(O)=O.[Na+]>O1CCCC1>[C:16]([NH:17][C@@H:18]1[C@@H:21]([O:24][CH2:25][C:26](=[O:35])[CH2:27][C:28]([O:30][C:31]([CH3:32])([CH3:34])[CH3:33])=[O:29])[NH:20][C:19]1=[O:23])(=[O:22])[C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=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 4

HCID 8000Boron trifluoride etherateHCID 516892Sodium BicarbonateHCID 13276951HCID 13276951、化合物HCID 13422882HCID 13422882、化合物

生成物 1

HCID 13422884HCID 13422884、化合物収率 31%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

30 ul of boron trifluoride etherate were added to a suspension of 216 mg (1.15 mmols) of (1R, 5S)-3-phenyl-4-oxa-2,6-diazabicyclo[3.2.0]hept-2-en-7-one and 400 mg (2.3 mmols) of freshly prepared tert.-butyl 4-hydroxyacetoacetate in 4 ml of anhydrous tetrahydrofuran at room temperature. After a short time a clear, light yellow solution formed, which was stirred for 0.5 hour at room temperature. It was then poured into dilute NaHCO3 solution. The mixture was extracted with methylene chloride, washed with water and dried over magnesium sulphate. After the solvent had been evaporated off in vacuo and the residue had been chromatographed on 60 g of silica gel (toluene:ethyl acetate 1:3), 128 mg (31%) of tert.-butyl 4-[3(R)-benzoylamino-2-azetidinon-4(R)-yloxy]acetoacetate were obtained as colorless crystals, melting point: 142° C., RF : 0.36 (toluene:ethyl acetate 1:4), [α]D20 =32.24° (0.955 percent in CHCl3).

後処理

  1. customAfter a short time a clear, light yellow solution formed
  2. extractionThe mixture was extracted with methylene chloride
  3. washwashed with water
  4. dry with materialdried over magnesium sulphate
  5. customAfter the solvent had been evaporated off in vacuo
  6. customthe residue had been chromatographed on 60 g of silica gel (toluene:ethyl acetate 1:3)

出典と根拠

ORDレコード
ord-d92833bab29f4ff4bc3b11da681e20b2
出典データセット
uspto-grants-1986_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04616084

反応ノート

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