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3-((Acetyloxy)methyl)-7-amino-8-oxo-5-thia-1-azabicyclo(4.2.0)oct-2-ene-2-carboxylic acid → 3-[(Acetyloxy)methyl]-7-[[(2,3-dihydro-5-benzofuranyl)-hydroxyacetyl]amino]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid

HRID 904022
ノート
印刷プレビュー

反応式

HRID 904022 の反応式
[OH:1][CH:2]([C:6]1[CH:7]=[CH:8][C:9]2[O:13][CH2:12][CH2:11][C:10]=2[CH:14]=1)[C:3]([OH:5])=O.C[Si](C([Si](C)(C)C)C(N)=O)(C)C.ClC(OCC(C)C)=O.[C:35]([O:38][CH2:39][C:40]1[CH2:47][S:46][CH:45]2[N:42]([C:43](=[O:49])[CH:44]2[NH2:48])[C:41]=1[C:50]([OH:52])=[O:51])(=[O:37])[CH3:36].C(=O)(O)[O-].[Na+]>O.C(OCC)(=O)C.CCOCC.C(N(CC)CC)C.C1COCC1>[C:35]([O:38][CH2:39][C:40]1[CH2:47][S:46][CH:45]2[N:42]([C:43](=[O:49])[CH:44]2[NH:48][C:3](=[O:5])[CH:2]([C:6]2[CH:7]=[CH:8][C:9]3[O:13][CH2:12][CH2:11][C:10]=3[CH:14]=2)[OH:1])[C:41]=1[C:50]([OH:52])=[O:51])(=[O:37])[CH3:36]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

11

反応物 5

HCID 137293-((Acetyloxy)methyl)-7-amino-8-oxo-5-thia-1-azabicyclo(4.2.0)oct-2-ene-2-carboxylic acidHCID 62365Isobutyl chloroformateHCID 516892Sodium BicarbonateHCID 11708267BistrimethylsilylacetamidHCID 233358212-(2,3-Dihydrobenzofuran-5-yl)-2-hydroxyacetic acid

生成物 1

HCID 23335848
3-[(Acetyloxy)methyl]-7-[[(2,3-dihydro-5-benzofuranyl)-hydroxyacetyl]amino]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid

試薬・触媒・溶媒 5

HCID 962Water溶媒2 回HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒2 回HCID 8471Triethylamine溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
-10 °C

実験手順

α-Hydroxy-(2,3-dihydro-5-benzofuranyl)acetic acid (10 mmole) triethylamine (10 mmole) and bistrimethylsilylacetamide (BSA) (10 mmole) are added to 50 ml of THF and refluxed for two hours. The reaction mixture is cooled to about -10° C. and 10 mmole of isobutyl chloroformate is added dropwise. After 30 minutes at -10° C., 10 mmole of 3-[(acetyloxy)methyl]-7-amino-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid in 50 ml of water--20 ml of THF containing 10 mmole of triethylamine is added dropwise to the cooled reaction mixture. The temperature is maintained between -10° C. and 0° C. during the addition. The reaction mixture is allowed to come to room temperature very slowly. About 50 cc of saturated aqueous sodium bicarbonate and 100 ml of water are added to the reaction mixture. This mixture is treated several times with ether which is then discarded. The aqueous phase is layered with ethyl acetate and the pH of the aqueous solution is adjusted to 1.5. The ethyl acetate is then separated from the aqueous phase, dried over magnesium sulfate, filtered and evaporated to give the title compound.

後処理

  1. temperaturerefluxed for two hours
  2. temperatureThe temperature is maintained between -10° C. and 0° C. during the addition
  3. customto come to room temperature
  4. customThe ethyl acetate is then separated from the aqueous phase
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated

出典と根拠

ORDレコード
ord-465e82eacbed49e6b67aed423f7e4b3c
出典データセット
uspto-grants-1980_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04229575

反応ノート

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