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

HRID 601092ノート

反応式

HRID 601092 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-58d0005d99bf4b80a0e98e4d6564161a
出典データセット
uspto-grants-2011_03
特許番号
US07902308B2

反応ノート

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