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Triethylamine → HCID 70096722、化合物

HRID 619704
ノート
印刷プレビュー

反応式

HRID 619704 の反応式
[CH2:1]([O:8][C:9]([N:11]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH2:13][CH:12]1[C:20]([OH:22])=O)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([N:25](CC)CC)C.ClC(OCC)=O.N[C@H:37]1[C@H:40]([O:41][C:42](=[O:44])[CH3:43])[NH:39][C:38]1=[O:45]>C(Cl)(Cl)Cl.C(OCC)(=O)C>[CH2:1]([O:8][C:9]([N:11]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH2:13][CH:12]1[C:20]([C@@H:37]1[C@H:40]([O:41][C:42](=[O:44])[CH3:43])[N:39]([NH2:25])[C:38]1=[O:45])=[O:22])=[O:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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

7

反応物 4

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 27764001-[(Benzyloxy)carbonyl]-2-indolinecarboxylic acidHCID 15428308HCID 15428308、化合物

生成物 1

HCID 70096722HCID 70096722、化合物収率 71%

試薬・触媒・溶媒 2

HCID 6212Chloroform
溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
-2.5 °C

実験手順

To a solution of 1-benzyloxycarbonyl-2-indoline carboxylic acid (320 mg, 1.05 mmol) and triethylamine (106 mg, 1.05 mmol) in chloroform (20 ml), ethyl chloroformate (109 mg, 1 mmol) was added at -15° C. The reaction mixture was stirred at a bath temperature of -10 to 5° C. for 1 hr. Then a precooled solution of (3S,4S)-3-amino-4-acetoxy-azetidin-2-one in ethyl acetate was added at -15° C. and stirring was continued at a bath temperature of -15 to 5° C. for 1 hr. After removal of solvent, the residue was dissolved in ethyl acetate, washed with water, brine and dried over sodium sulfate. After removal of solvent, the residue was purified by silica gel column chromatography using hexane-ethyl acetate (1:3) as eluent and the title compound was obtained.

後処理

  1. stirringstirring
  2. customwas continued at a bath
  3. waittemperature of -15 to 5° C. for 1 hr
  4. customAfter removal of solvent
  5. dissolutionthe residue was dissolved in ethyl acetate
  6. washwashed with water, brine
  7. dry with materialdried over sodium sulfate
  8. customAfter removal of solvent
  9. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-dcb480c362444f43a6970770ca97fa55
出典データセット
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05959123

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート