Water → 2,4-Bis(tert-butyl)-6-[[(2,6-dibromophenyl)amino]methyl]phenol

HRID 601092노트

반응식

HRID 601092 반응식
[C:1]([C:5]1[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:8]=[C:7]([CH:15]=[N:16][C:17]2[C:22]([Br:23])=[CH:21][CH:20]=[CH:19][C:18]=2[Br:24])[C:6]=1[OH:25])([CH3:4])([CH3:3])[CH3:2].[BH4-].[Na+].O>CO>[C:1]([C:5]1[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:8]=[C:7]([CH2:15][NH:16][C:17]2[C:22]([Br:23])=[CH:21][CH:20]=[CH:19][C:18]=2[Br:24])[C:6]=1[OH:25])([CH3:2])([CH3:3])[CH3:4]

참가 물질

5

반응물 3

HCID 962WaterHCID 4311764Sodium borohydrideHCID 1363467102,4-Bis(tert-butyl)-6-[[(2,6-dibromophenyl)imino]methyl]phenol

생성물 1

HCID 866276672,4-Bis(tert-butyl)-6-[[(2,6-dibromophenyl)amino]methyl]phenol

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a suspension of 2,4-bis(tert-butyl)-6-[[(2,6-dibromophenyl)imino]methyl]phenol (0.91 g, 2.41 mmol) in methanol (20 ml) was added NaBH4 (1.2 g), in small portions. The yellow suspension was stirred for 2 hours during which the yellow solution turned clear. Water (10 ml) was then slowly added, the organic phase separated and the aqueous phase extracted with dichloromethane (3×10 ml). The organic fractions were combined, dried (NaSO4), and the solvent removed under reduced pressure. The crude product was purified by recrystallisation from hot hexane to afford the product as large colourless crystals. Yield 0.48 g, 95%.

후처리

  1. customthe organic phase separated
  2. extractionthe aqueous phase extracted with dichloromethane (3×10 ml)
  3. dry with materialdried (NaSO4)
  4. customthe solvent removed under reduced pressure
  5. customThe crude product was purified by recrystallisation from hot hexane

출처 및 근거

ORD 기록
ord-58d0005d99bf4b80a0e98e4d6564161a
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07902308B2

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