Trifluoroacetic acid → H-Thz-NH-tBu

반응식

[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]

참가 물질

반응물 2

HCID 6422Trifluoroacetic acid

HCID 54130109Boc-Thz-NH-tBu

생성물 1

HCID 10535636H-Thz-NH-tBu수율 94%

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록: ord-a6311746ebb44617980e9d996fa55ecc
출처 데이터셋: uspto-grants-1997_07
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US05644028

반응 노트

불러오는 중…