Sodium borohydride → 3,5-dichloro-4-hydroxymethyl-N-methylaniline

HRID 1290167노트

반응식

HRID 1290167 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([Cl:12])[C:9]=1[CH:10]=[O:11])[NH:5][CH3:6].[BH4-].[Na+]>CO.O1CCCC1>[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([Cl:12])[C:9]=1[CH2:10][OH:11])[NH:5][CH3:6]

참가 물질

5

반응물 2

HCID 4311764Sodium borohydrideHCID 18923365HCID 18923365, 화합물

생성물 1

HCID 189235483,5-dichloro-4-hydroxymethyl-N-methylaniline수율 100.7%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 3,5-dichloro-4-formyl-N-methylaniline (242 mg) in methanol (3 ml) and tetrahydrofuran (3 ml) was added sodium borohydride (45 mg) and the mixture was stirred for 30 minutes at ambient temperature. The reaction mixture was quenched with aqueous saturated ammonium chloride solution and ethyl acetate was added thereto. The separated organic layer was washed with aqueous saturated ammonium chloride solution, dried and concentrated in vacuo to give 3,5-dichloro-4-hydroxymethyl-N-methylaniline (246 mg).

후처리

  1. customThe reaction mixture was quenched with aqueous saturated ammonium chloride solution and ethyl acetate
  2. additionwas added
  3. washThe separated organic layer was washed with aqueous saturated ammonium chloride solution
  4. customdried
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-af329abe7e2f445ba79cfc209a513b35
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05750699

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