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1-Hydroxybenzotriazole → 1,1-Dimethylethyl 4-[(6-bromo-1,2-benzisoxazol-3-yl)acetyl]-1-piperazinecarboxylate

HRID 1988891
ノート
印刷プレビュー

反応式

HRID 1988891 の反応式
[Br:1][C:2]1[CH:14]=[CH:13][C:5]2[C:6]([CH2:9][C:10]([OH:12])=O)=[N:7][O:8][C:4]=2[CH:3]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.ON1C2C=CC=CC=2N=N1.[N:49]1([C:55]([O:57][C:58]([CH3:61])([CH3:60])[CH3:59])=[O:56])[CH2:54][CH2:53][NH:52][CH2:51][CH2:50]1>O1CCCC1>[Br:1][C:2]1[CH:14]=[CH:13][C:5]2[C:6]([CH2:9][C:10]([N:52]3[CH2:51][CH2:50][N:49]([C:55]([O:57][C:58]([CH3:61])([CH3:60])[CH3:59])=[O:56])[CH2:54][CH2:53]3)=[O:12])=[N:7][O:8][C:4]=2[CH:3]=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 757711-HydroxybenzotriazoleHCID 143452tert-Butyl piperazine-1-carboxylateHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 591273762-(6-Bromo-1,2-benzoxazol-3-yl)acetic acid2 回

生成物 1

HCID 586564751,1-Dimethylethyl 4-[(6-bromo-1,2-benzisoxazol-3-yl)acetyl]-1-piperazinecarboxylate
収率 98.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A suspension of (6-bromo-1,2-benzisoxazol-3-yl)acetic acid (Intermediate 32) (0.06 g) and HATU (0.09 g) in dry tetrahydrofuran (2 ml) was stirred at room temp. for 5 min. 1-Hydroxybenzotriazole (0.03 g) and 1,1-dimethylethyl 1-piperazinecarboxylate (0.04 g) were added and the reaction mixture was stirred for a further 18 h. The solvent was removed under vacuum and the residue was partitioned between dichloromethane and 2N aqueous sodium carbonate. The layers were separated and the organic layer was applied to a Varian Bond-Elut SPE cartridge (silica, 5 g ) eluting sequentially with dichloromethane, chloroform, ether and ethyl acetate to give the title compound as a white solid (0.09 g).

後処理

  1. stirringthe reaction mixture was stirred for a further 18 h
  2. customThe solvent was removed under vacuum
  3. customthe residue was partitioned between dichloromethane and 2N aqueous sodium carbonate
  4. customThe layers were separated
  5. washeluting sequentially with dichloromethane, chloroform, ether and ethyl acetate

出典と根拠

ORDレコード
ord-d84edfba34144f8c92338cbc8e5bb4b2
出典データセット
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07642276B2

反応ノート

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