Sodium Hydroxide → HCID 68879751、化合物

HRID 1454236ノート

反応式

HRID 1454236 の反応式
[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]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 4311764Sodium borohydrideHCID 86618491HCID 86618491、化合物

生成物 1

HCID 68879751HCID 68879751、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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]+.

後処理

  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%)

出典と根拠

ORDレコード
ord-ab3b07f3bc5a4362a69ba85742ef8077
出典データセット
uspto-grants-2009_01
特許番号
US07479493B2

反応ノート

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