Triethylamine → HCID 12944618, 화합물

HRID 649088노트

반응식

HRID 649088 반응식
[NH:1]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[C@H:2]([C:6]([O:8]N1C(=O)CCC1=O)=O)[CH:3]([CH3:5])[CH3:4].[NH2:23][C@H:24]([C:40]([O:42][CH3:43])=[O:41])[CH2:25][CH2:26][CH2:27][CH2:28][NH:29][C:30]([O:32][CH2:33][C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1)=[O:31].Cl.C(N(CC)CC)C>C1COCC1>[NH:1]([C:16]([O:18][C:19]([CH3:20])([CH3:21])[CH3:22])=[O:17])[C@H:2]([C:6]([NH:23][C@H:24]([C:40]([O:42][CH3:43])=[O:41])[CH2:25][CH2:26][CH2:27][CH2:28][NH:29][C:30]([O:32][CH2:33][C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1)=[O:31])=[O:8])[CH:3]([CH3:4])[CH3:5]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 98768Boc-Val-osuHCID 12935371H-Lys(Z)-OMe HCl

생성물 1

HCID 12944618HCID 12944618, 화합물수율 99.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of t-Boc-Val-OSu (3.14 g, 10 mmol) and H-Lys(CBZ)-OCH3.HCl (3.31 g, 10 mmol) in THF (300 ml) was treated at room temperature with triethylamine (1.38 ml) and left stirring for 17 hr. The resulting solution was evaporated in vacuo and the residue was dissolved in EtOAc (500 ml). The organic solution was washed successively with water (2×200 ml), 5% citric acid (2×200 ml), water (2×200 ml) and dried over Na2SO4. The dried solution was filtered and evaporated in vacuo to give (VI) (4.9 g; 99%) as a foam. T.l.c. RfE4 =0.64.

후처리

  1. waitleft
  2. customThe resulting solution was evaporated in vacuo
  3. dissolutionthe residue was dissolved in EtOAc (500 ml)
  4. washThe organic solution was washed successively with water (2×200 ml), 5% citric acid (2×200 ml), water (2×200 ml)
  5. dry with materialdried over Na2SO4
  6. filtrationThe dried solution was filtered
  7. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-41cf3b78fcb148b582cc1f92fa0a07a1
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04737487

반응 노트

불러오는 중…