Sodium Hydroxide → HCID 57079581, 화합물

HRID 439843노트

반응식

HRID 439843 반응식
[CH3:1][C:2]1[CH:10]=[CH:9][C:8]2[NH:7][C:6]3[C:11]4[C:16]([CH2:17][C:5]=3[C:4]=2[CH:3]=1)=[CH:15][CH:14]=[CH:13][CH:12]=4.C([BH3-])#N.[Na+].[OH-].[Na+]>C(O)(=O)C>[CH3:1][C:2]1[CH:10]=[CH:9][C:8]2[NH:7][C@@H:6]3[C:11]4[C:16]([CH2:17][C@@H:5]3[C:4]=2[CH:3]=1)=[CH:15][CH:14]=[CH:13][CH:12]=4

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 5003444Sodium cyanoborohydrideHCID 222470798-Methyl-5,10-dihydroindeno[1,2-b]indole

생성물 1

HCID 57079581HCID 57079581, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

5,10-Dihydro-8-methylindeno[1,2-b]indole (10 g, 46 mmol) was stirred at room temperature in glacial acetic acid (150 cm3). Sodium cyanoborohydride (8.6 g, 3 equivalents) was added portionwise over a period of 30 minutes. The reaction was stirred for a further hour, and then poured into ice/water (200 cm3). After stirring for 30 minutes, the acidic solution was made basic by the addition of sodium hydroxide, and the colourless solid thus formed collected by filtration. This solid was washed copiously with water until the residue was free from cyanide ion, and then dried in a vacuum oven to yield the title compound as a colourless solid. Yield: 7.5 g (73%) M.p. 110° C. (from ethanol/water). 1H NMR (CDCl3) δ: 2.24 (3H, s,), 3.20 (1H, dd,), 3.50 (1H, dd,) 3.9 (1H, br,), 4.16 (1H, dd,), 5.23 (1H, d,), 6.52 (1H,d,), 6.80 (1H, d,), 6.99 (1H, s,), 7.1-7.4 (4H, m,).

후처리

  1. stirringAfter stirring for 30 minutes
  2. customthe colourless solid thus formed
  3. filtrationcollected by filtration
  4. washThis solid was washed copiously with water until the residue
  5. customdried in a vacuum oven

출처 및 근거

ORD 기록
ord-ca0f4c6f72a8490da954a345f5cf53e7
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05516788

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