Ammonium Chloride → (2,3-Dichloro-6-nitrophenyl)methanol

HRID 731677

反応式

HRID 731677 の反応式
[Cl:1][C:2]1[C:9]([Cl:10])=[CH:8][CH:7]=[C:6]([N+:11]([O-:13])=[O:12])[C:3]=1[CH:4]=[O:5].[BH4-].[Na+].[Cl-].[NH4+]>CO>[Cl:1][C:2]1[C:9]([Cl:10])=[CH:8][CH:7]=[C:6]([N+:11]([O-:13])=[O:12])[C:3]=1[CH2:4][OH:5]

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 4311764Sodium borohydrideHCID 112182712,3-Dichloro-6-nitrobenzaldehyde

生成物 1

HCID 11160370(2,3-Dichloro-6-nitrophenyl)methanol収率 91.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

196MBT36 (100 mg, 0.455 mmol) was dissolved in methanol (2 mL). Sodium borohydride (17 mg, 0.455 mmol) was added and the mixture was stirred for 30 minutes at room temperature. Saturated aqueous ammonium chloride (1 mL) was added and extracted with dichloromethane (2×10 mL). The combined organic phases were dried over Na2SO4, filtered and evaporated to give 2,3-dichloro-6-nitrobenzyl alcohol (196MBT46-A, 92 mg, 91%) as a yellow solid.

後処理

  1. extractionextracted with dichloromethane (2×10 mL)
  2. dry with materialThe combined organic phases were dried over Na2SO4
  3. filtrationfiltered
  4. customevaporated

出典と根拠

ORDレコード
ord-40beb7fda9d44a468b721181526bd306
出典データセット
uspto-grants-2009_09
特許番号
US07585877B2

関連ノート

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