4-Methylmorpholine → HCID 10636385, 화합물

HRID 1593305노트

반응식

HRID 1593305 반응식
[NH2:1][C@@H:2]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[C:3]([O:5][CH3:6])=[O:4].Cl.[OH:14][C@@H:15]([CH2:19][CH:20]([CH3:22])[CH3:21])[C:16](O)=[O:17].CN1CCOCC1.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.Cl>ClCCl>[OH:14][C@@H:15]([CH2:19][CH:20]([CH3:22])[CH3:21])[C:16]([NH:1][C@@H:2]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[C:3]([O:5][CH3:6])=[O:4])=[O:17]

참가 물질

7

반응물 5

HCID 79724-Methylmorpholine2회HCID 757711-HydroxybenzotriazoleHCID 1201451Methyl phenylglycinate, L-HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 86604641HCID 86604641, 화합물

생성물 1

HCID 10636385HCID 10636385, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a cooled (0° C.) solution of methyl (2S)-amino(phenyl)acetate (3.06 g), (2S)-2-hydroxy-4-methylpentanoic acid hydrochloride, NMM (1.85 ml), and HOBt (6.15 g) in dichloromethane (50 ml) was added EDAC-HCl (5.81 g). Additional NMM (2.31 ml) was then added. The mixture was stirred for 2h at 0° C., then overnight at RT. The reaction was concentrated and the residue was taken up in Ethyl acetate washed with 0.1N hydrochloric acid, saturated sodium bicarbonate, brine, dried, filtered and evaporated to afford the title compound (4.20 g). 1H NMR (300 MHz, CDCl3) δ 0.92-0.95 (m, 6H), 1.47-1.67 (m, 2H), 1.76-2.04 (m, 1H), 2.63 (bs, 1H), 3.74 (s, 3H), 4.21 (d, 1H, J=9 Hz), 5.58 (d, 1H, J=8 Hz), 7.26-7.42 (m, 5H). MS APCI, m/z=280 (M+1). LC/MS: 1.95 min.

후처리

  1. customovernight
  2. customat RT
  3. concentrationThe reaction was concentrated
  4. washwashed with 0.1N hydrochloric acid, saturated sodium bicarbonate, brine
  5. customdried
  6. filtrationfiltered
  7. customevaporated

출처 및 근거

ORD 기록
ord-3e251dffe6cb43b6a6f3f00c516c0a38
출처 데이터셋
uspto-grants-2007_11
특허 번호
US07294622B2

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