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Diisopropylethylamine → HCID 172983304, 화합물

HRID 515653
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HRID 515653 반응식
[CH2:1]1[S:5][C@@H:4]([CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][C:11]([OH:13])=[O:12])[C@H:3]2[NH:14][C:15]([NH:17][C@@H:2]12)=[O:16].O[N:19]=[C:20]([NH2:36])[CH2:21][CH2:22][CH2:23][CH2:24][N:25]1[C:29]2[CH:30]=[C:31]([CH3:34])[CH:32]=[CH:33][C:28]=2[O:27][C:26]1=[O:35].CCN=C=NCCCN(C)C.Cl.CCN(C(C)C)C(C)C>CN(C=O)C.ClCCl>[O:16]=[C:15]1[NH:17][C@H:2]2[CH2:1][S:5][C@@H:4]([CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][C:11]([O:13]/[N:19]=[C:20](\[NH2:36])/[CH2:21][CH2:22][CH2:23][CH2:24][N:25]3[C:29]4[CH:30]=[C:31]([CH3:34])[CH:32]=[CH:33][C:28]=4[O:27][C:26]3=[O:35])=[O:12])[C@H:3]2[NH:14]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 81531DiisopropylethylamineHCID 446904HCID 446904, 화합물HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 123617581HCID 123617581, 화합물

생성물 1

HCID 172983304HCID 172983304, 화합물수율 91.6%

시약·촉매·용매 2

HCID 6228
Dimethylformamide
용매
HCID 6344Dichloromethane용매

실험 절차

To a suspension of homobiotin 83 (10 mg, 0.039 mmol) and compound 13 (11 mg, 0.043 mmol) in anhydrous DMF (0.5 ml) was added EDCl (7 mg, 0.047 mmol) and DIPEA (6 mg, 0.045 mmol) and stirred under a nitrogen atmosphere at ambient temperature for 12 h. The reaction mixture was diluted with dichloromethane (25 ml) and washed with water (25 ml) and brine (25 ml). The organic layer was dried over sodium sulphate, filtered and concentrated in vacuo. The residue was purified by silica gel chromatography eluting with 19:1 dichloromethane/methanol to give a yellow oil (18 mg, 46%).

후처리

  1. washwashed with water (25 ml) and brine (25 ml)
  2. dry with materialThe organic layer was dried over sodium sulphate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by silica gel chromatography
  6. washeluting with 19:1 dichloromethane/methanol

출처 및 근거

ORD 기록
ord-55d4529ce9d849b99e4515ef93061b8c
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09108978B2

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