Trifluoroacetic acid → H-Thz-NH-tBu

反応式

[N:1]1(C(OC(C)(C)C)=O)[CH2:12][S:11][CH2:10][C@H:2]1[C:3]([NH:5][C:6]([CH3:9])([CH3:8])[CH3:7])=[O:4].FC(F)(F)C(O)=O>>[NH:1]1[CH2:12][S:11][CH2:10][C@H:2]1[C:3]([NH:5][C:6]([CH3:9])([CH3:7])[CH3:8])=[O:4]

参加物

反応物 2

HCID 6422Trifluoroacetic acid

HCID 54130109Boc-Thz-NH-tBu

生成物 1

HCID 10535636H-Thz-NH-tBu収率 94%

実験手順

To 3.25 g (11.3 mmol) of Boc-Thz-NH-tBu, 15 ml (195 mmol) of trifluoroacetic acid was added under ice cooling and the resultant mixture was stirred at that temperature for 30 min and evaporated. The residue was washed with hexane by decantation and partitioned between chloroform and 1N NaOH aqueous solution. The organic layer was dried over Na2SO4 and evaporated under reduced pressure to give 2.00 g (Y. 94%) of H-Thz-NH-tBu which was convened to Qoa--Mta--AHPBA--Thz--NH-tBu by a similar method with processes 3-5 of Example 3.

後処理

customevaporated
washThe residue was washed with hexane by decantation
custompartitioned between chloroform and 1N NaOH aqueous solution
dry with materialThe organic layer was dried over Na2SO4
customevaporated under reduced pressure

出典と根拠

ORDレコード: ord-a6311746ebb44617980e9d996fa55ecc
出典データセット: uspto-grants-1997_07
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US05644028

反応ノート

読み込み中…

参加物