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Diisopropylethylamine → 2-(4-Ethoxy-3-methoxy-phenyl)-N-{2-[2-methyl-6-(2,4,6-trimethyl-phenylamino)-pyrimidin-4-ylamino]ethyl}-acetamide

HRID 1634570
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HRID 1634570 반응식
[NH2:1][CH2:2][CH2:3][NH:4][C:5]1[CH:10]=[C:9]([NH:11][C:12]2[C:17]([CH3:18])=[CH:16][C:15]([CH3:19])=[CH:14][C:13]=2[CH3:20])[N:8]=[C:7]([CH3:21])[N:6]=1.[CH2:22]([O:24][C:25]1[CH:33]=[CH:32][C:28]([CH2:29][CH2:30]N)=[CH:27][C:26]=1[O:34][CH3:35])[CH3:23].C(N(CC)C(C)C)(C)C.F[P-](F)(F)(F)(F)F.N1([O:61][P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1>C(Cl)Cl>[CH2:22]([O:24][C:25]1[CH:33]=[CH:32][C:28]([CH2:29][C:30]([NH:1][CH2:2][CH2:3][NH:4][C:5]2[CH:10]=[C:9]([NH:11][C:12]3[C:17]([CH3:18])=[CH:16][C:15]([CH3:19])=[CH:14][C:13]=3[CH3:20])[N:8]=[C:7]([CH3:21])[N:6]=2)=[O:61])=[CH:27][C:26]=1[O:34][CH3:35])[CH3:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 81531DiisopropylethylamineHCID 1420764-Ethoxy-3-methoxyphenethylamineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 22034099(2-Aminoethyl){2-methyl-6-[(2,4,6-trimethylphenyl)amino]pyrimidin-4-yl}amine

생성물 1

HCID 220341212-(4-Ethoxy-3-methoxy-phenyl)-N-{2-[2-methyl-6-(2,4,6-trimethyl-phenylamino)-pyrimidin-4-ylamino]ethyl}-acetamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of (2-aminoethyl){2-methyl-6-[(2,4,6-trimethylphenyl)amino]pyrimidin-4-yl}amine (0.36 g, 1.26 mmol), 4-ethoxy-3-methoxyphenethylamine (0.26 g, 1.26 mmol)) and N,N diisopropylethyl amine (0.24 ml, 1.38 mmol in CH2Cl2 (5 mL), add benzotriazol-1-yloxytris-(dimethylamino)phosphonium hexafluorophosphate (0.61 g, 1.38 mmol) and stir at ambient temperature for 14 h. Dilute the resulting mixture with CH2Cl2 (20 mL), and wash with water (20 mL) and saturated aq NaCl (20 mL). Dry the organic layer over Na2SO4, filter and concentrate in vacuo. Purify by preparative TLC (7% methanol-CH2Cl2) to obtain the title compound.

후처리

  1. washwash with water (20 mL) and saturated aq NaCl (20 mL)
  2. dry with materialDry the organic layer over Na2SO4
  3. filtrationfilter
  4. concentrationconcentrate in vacuo
  5. customPurify by preparative TLC (7% methanol-CH2Cl2)

출처 및 근거

ORD 기록
ord-fb699aff5e504c4ea8f48476d39f1a24
출처 데이터셋
uspto-grants-2003_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06506762B1

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