Methyl iodide → HCID 9836515, 화합물

HRID 448655노트

반응식

HRID 448655 반응식
[NH2:1][C:2]1[N:3]=[C:4]([Cl:20])[C:5]2[CH:10]=[CH:9][N:8]([C@@H:11]3[O:17][C@H:16]([CH2:18][OH:19])[C@@H:14]([OH:15])[C@H:12]3[OH:13])[C:6]=2[N:7]=1.[H-].[Na+].I[CH3:24]>CN(C=O)C>[NH2:1][C:2]1[N:3]=[C:4]([Cl:20])[C:5]2[CH:10]=[CH:9][N:8]([C@@H:11]3[O:17][C@H:16]([CH2:18][OH:19])[C@@H:14]([OH:15])[C@H:12]3[O:13][CH3:24])[C:6]=2[N:7]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 11174104HCID 11174104, 화합물

생성물 1

HCID 9836515HCID 9836515, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of the compound from Step B (1.0 g, 3.3 mmol) in dry DMF (100 mL) at 15° C. was treated with 60% NaH (0.14 g, 3.5 mmol). After 30 min., iodomethane (47 g, 3.3 mmol) was added portionwise to the stirred solution. The reaction was stirred at room temperature for 16 hrs. and then evaporated at a temperature below 40° C. The resulting solid was chromatographed on silica gel to afford the product as a white solid; yield 0.81 g. 1H NMR (DMSO-d6): δ 3.25 (s, 3H), 3.54 (m, 2H), 3.87 (m, 1H), 4.07 (m, 1H), 4.22 (m, 1H), 5.01 (m, 1H), 5.16 (d, 1H), 6.07 (d, 1H), 6.37 (d, 1H), 6.70 (s br, 2H), 7.40 (s, 1H). Mass spectrum: m/z 316 (M+1)+.

후처리

  1. customand then evaporated at a temperature below 40° C
  2. customThe resulting solid was chromatographed on silica gel

출처 및 근거

ORD 기록
ord-4eddfe13095d4752a3a023966081ca1c
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08481712B2

반응 노트

불러오는 중…