반응식
[NH2:1][C@H:2]([CH2:8][CH2:9][CH2:10][CH2:11][NH:12][C:13]([O:15][CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)=[O:14])[C:3]([O:5][CH2:6][CH3:7])=[O:4].[C:23]([N:27]=[C:28]=[S:29])([CH3:26])([CH3:25])[CH3:24].[N-]=C=S>C(O)C.CCOCC>[CH2:16]([O:15][C:13]([NH:12][CH2:11][CH2:10][CH2:9][CH2:8][C@@H:2]([NH:1][C:28]([NH:27][C:23]([CH3:26])([CH3:25])[CH3:24])=[S:29])[C:3]([O:5][CH2:6][CH3:7])=[O:4])=[O:14])[C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1참가 물질
반응물 3
생성물 1
시약·촉매·용매 2
반응 조건
- 온도
- 80 °C
실험 절차
The process is performed as in Example 2, starting with 7.4 g of ethyl (2R)-2-amino-6-{[(benzyloxy)carbonyl]-amino}hexanoate with 5 cm3 of tert-butyl isothiocyanate in 200 cm3 of anhydrous ethanol at a temperature in the region of 20° C. for 20 hours. The reaction is completed by addition of a further 1 cm3 of isothiocyanate and heating for 2 hours at a temperature in the region of 80° C. The reaction medium is concentrated under reduced pressure (5 kPa) at a temperature in the region of 40° C. The residue obtained is taken up in ether and concentrated again under the above conditions. 13 g of ethyl (2R)-6-{[(benzyloxy)carbonyl]amino}-2-{[(tert-butylamino)carbothioyl]amino}hexanoate are obtained in the form of a colorless oil. (αD20=−12.5±0.5 at a concentration of 0.5% in methanol).
후처리
- concentrationThe reaction medium is concentrated under reduced pressure (5 kPa) at a temperature in the region of 40° C
- customThe residue obtained
- concentrationconcentrated again under the above conditions
출처 및 근거
- ORD 기록
- ord-28959d29fab34f3faafa931b30da8b88
- 출처 데이터셋
- uspto-grants-2004_03
- 특허 번호
- US06699895B2
연결된 노트
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