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Sodium Hydroxide → HCID 69210030、化合物

HRID 2214240
ノート
印刷プレビュー

反応式

HRID 2214240 の反応式
C([O:3][C:4](=[O:37])[CH:5]([CH2:14][CH2:15][CH2:16][S:17][C:18]([C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH2:6][C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])C.[OH-].[Na+]>CO.O>[C:10]([O:9][C:7](=[O:8])[CH2:6][CH:5]([CH2:14][CH2:15][CH2:16][S:17][C:18]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)([C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1)[C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)[C:4]([OH:37])=[O:3])([CH3:13])([CH3:11])[CH3:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 69211802HCID 69211802、化合物

生成物 1

HCID 69210030HCID 69210030、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of the compound of example 28 (3.00 g, 5.78 mmol) in methanol (30 mL) and water (10 mL) was added NaOH (1N, 11.6 mL, 11.6 mmol). The mixture was stirred vigorously under ambient conditions. After 24 hours, most of the methanol has evaporated. The residue was portioned between water and ether. The water phase was extracted two times with ether, then acidified with HCl (1N) to pH 1. The water phase was extracted three times with ethyl acetate. The recombined organic phase was dried over sodium sulfate, filtered, and evaporated. The residue was flashed using 5% methanol in chloroform to give the product as a white solid. 1H-NMR(CDCl3, 400 MH: 1.45(s, 9H); 1.35–1.64(m, 4H); 1.58(m, 1H); 2.16(m, 2H); 2.26(m, 1H); 2.64(m, 1H); 4.12(q, J=7.1 Hz, 2H), 7.19–7.29, 7.40(m, 15H).

後処理

  1. custommost of the methanol has evaporated
  2. extractionThe water phase was extracted two times with ether
  3. extractionThe water phase was extracted three times with ethyl acetate
  4. dry with materialThe recombined organic phase was dried over sodium sulfate
  5. filtrationfiltered
  6. customevaporated

出典と根拠

ORDレコード
ord-9147cb75a0fe44d581049af8512bf071
出典データセット
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07105539B2

反応ノート

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