Sodium Hydroxide → HCID 68879751, 화합물

HRID 1454236노트

반응식

HRID 1454236 반응식
[C:1]([O:5][C:6](=[O:27])[N:7]([CH2:9][C:10]1[CH:15]=[C:14]([CH:16]=[O:17])[CH:13]=[CH:12][C:11]=1[O:18][C:19]1[CH:24]=[CH:23][C:22]([Cl:25])=[C:21]([Cl:26])[CH:20]=1)[CH3:8])([CH3:4])([CH3:3])[CH3:2].[BH4-].[Na+].[OH-].[Na+]>CO>[C:1]([O:5][C:6](=[O:27])[N:7]([CH2:9][C:10]1[CH:15]=[C:14]([CH2:16][OH:17])[CH:13]=[CH:12][C:11]=1[O:18][C:19]1[CH:24]=[CH:23][C:22]([Cl:25])=[C:21]([Cl:26])[CH:20]=1)[CH3:8])([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 4311764Sodium borohydrideHCID 86618491HCID 86618491, 화합물

생성물 1

HCID 68879751HCID 68879751, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of [2-(3,4-dichloro-phenoxy)-5-formyl-benzyl]-methyl-carbamic acid tert-butyl ester (816 mg, 1.98 mmol) in MeOH (40 mL), was added NaBH4 (75 mg, 1.98 mmol). After 24 h, the mixture was treated with 1 N NaOH, was stirred an additional 1 h, and then partially concentrated. The resulting aqueous mixture was extracted with DCM and the combined organic layers were dried (Na2SO4) and concentrated. The crude material was carried forward without further purification (784 mg, 96%). MS (ESI): mass calcd. for C20H23Cl2NO4, 411.10; m/z found, 434.7 [M+Na]+.

후처리

  1. concentrationpartially concentrated
  2. extractionThe resulting aqueous mixture was extracted with DCM
  3. dry with materialthe combined organic layers were dried (Na2SO4)
  4. concentrationconcentrated
  5. customThe crude material was carried forward without further purification (784 mg, 96%)

출처 및 근거

ORD 기록
ord-ab3b07f3bc5a4362a69ba85742ef8077
출처 데이터셋
uspto-grants-2009_01
특허 번호
US07479493B2

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