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Acetic Acid → 4-tert-butyl 6-methyl (6R,7R)-7-(3,4-dichlorophenyl)-1,4-oxazepane-4,6-dicarboxylate

HRID 1022679
ノート
印刷プレビュー

反応式

HRID 1022679 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:14][C@@H:13]([C:15]([OH:17])=[O:16])[C@H:12]([C:18]2[CH:23]=[CH:22][C:21]([Cl:24])=[C:20]([Cl:25])[CH:19]=2)[O:11][CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH3:26][Si](C=[N+]=[N-])(C)C.C(O)(=O)C>C1(C)C=CC=CC=1.CO>[Cl:25][C:20]1[CH:19]=[C:18]([C@@H:12]2[O:11][CH2:10][CH2:9][N:8]([C:6]([O:5][C:1]([CH3:4])([CH3:2])[CH3:3])=[O:7])[CH2:14][C@H:13]2[C:15]([O:17][CH3:26])=[O:16])[CH:23]=[CH:22][C:21]=1[Cl:24]
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 3

HCID 176Acetic AcidHCID 167693TrimethylsilyldiazomethaneHCID 66975341(6R,7R)-4-(tert-butoxycarbonyl)-7-(3,4-dichlorophenyl)-1,4-oxazepane-6-carboxylic acid

生成物 1

HCID 866638664-tert-butyl 6-methyl (6R,7R)-7-(3,4-dichlorophenyl)-1,4-oxazepane-4,6-dicarboxylate

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 1140
Toluene
溶媒

実験手順

To a mixed solution of (6R,7R)-4-(tert-butoxycarbonyl)-7-(3,4-dichlorophenyl)-1,4-oxazepane-6-carboxylic acid (0.82 g) in toluene (10 ml) and methanol (2 mL) was added trimethylsilyldiazomethane (1.576 mL, 2 mol/l hexane solution) at 0° C. and the mixture was stirred for 30 min. Acetic acid was added until the solution became colorless. The solvent was evaporated under reduced pressure, and the residue was extracted with ethyl acetate and water. The organic layer was washed with brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure to give the title compound (0.51 g).

後処理

  1. customThe solvent was evaporated under reduced pressure
  2. extractionthe residue was extracted with ethyl acetate and water
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-7a057b0da6af43a19026b3f4308b5e4f
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08722662B2

反応ノート

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