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Sodium Hydroxide → tert-Butyl 3-thioureidopropylcarbamate

HRID 1755461
ノート
印刷プレビュー

反応式

HRID 1755461 の反応式
C([NH:9][C:10](=[S:23])[NH:11][CH2:12][CH2:13][CH2:14][NH:15][C:16](=[O:22])[O:17][C:18]([CH3:21])([CH3:20])[CH3:19])(=O)C1C=CC=CC=1.[OH-].[Na+]>CO>[NH:11]([CH2:12][CH2:13][CH2:14][NH:15][C:16](=[O:22])[O:17][C:18]([CH3:20])([CH3:19])[CH3:21])[C:10]([NH2:9])=[S:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 14280415tert-Butyl 3-(3-benzoylthioureido)propylcarbamate

生成物 1

HCID 20616909tert-Butyl 3-thioureidopropylcarbamate収率 72%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of material from Example 58 (6.89 g, 20.43 mmol) in MeOH (40 mL) is slowly added aqueous 5M NaOH (4.49 mL, 22.47 mmol) and the reaction is allowed to stir for 1 h at room temp. The solvent is removed in vacuo, the residue is neutralized with acetic acid and partitioned between water and EtOAc. The water layer is extracted with EtOAC, the organic layers are combined, washed with brine, dried over Na2SO4, filtered and evaporated to dryness to give 3.43 g (50.2%) of the title compound. LC/MS (Condition A): ret. T=2.54 min, (M+Na) 256.13.

後処理

  1. customThe solvent is removed in vacuo
  2. custompartitioned between water and EtOAc
  3. extractionThe water layer is extracted with EtOAC
  4. washwashed with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. customevaporated to dryness

出典と根拠

ORDレコード
ord-afabd929efe7455c8ee92fb226c440aa
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09169295B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート