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tert-Butanol → HCID 68997226、化合物

HRID 660763
ノート
印刷プレビュー

反応式

HRID 660763 の反応式
Cl[S:2]([N:5]=[C:6]=[O:7])(=[O:4])=[O:3].[C:8]([OH:12])([CH3:11])([CH3:10])[CH3:9].[CH3:13][Si:14]([CH3:43])([CH3:42])[CH2:15][CH2:16][O:17][C:18](=[O:41])[CH2:19][O:20][C:21]1[CH:26]=[CH:25][C:24]([NH:27][CH2:28][C:29]([O:31][CH3:32])=[O:30])=[C:23]([O:33][CH2:34][C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[CH:22]=1.C(N(CC)CC)C>C(Cl)Cl>[CH2:34]([O:33][C:23]1[CH:22]=[C:21]([O:20][CH2:19][C:18](=[O:41])[O:17][CH2:16][CH2:15][Si:14]([CH3:42])([CH3:43])[CH3:13])[CH:26]=[CH:25][C:24]=1[N:27]([S:2]([NH:5][C:6]([O:12][C:8]([CH3:11])([CH3:10])[CH3:9])=[O:7])(=[O:4])=[O:3])[CH2:28][C:29]([O:31][CH3:32])=[O:30])[C:35]1[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6386tert-ButanolHCID 8471TriethylamineHCID 70918Chlorosulfonyl isocyanateHCID 68838279HCID 68838279、化合物

生成物 1

HCID 68997226HCID 68997226、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

反応条件

温度
0 °C

実験手順

To an ice cooled solution of chlorosulfonyl isocyanate (2.55 g, 18 mmol) in methylene chloride (50 mL) is added dropwise a solution of t-butanol (1.33 g, 18 mmol) in methylene chloride (5 mL). The mixture is allowed to wart to RT, stirred for 15 min then re-chilled to 0° C. To this is added dropwise a solution of [3-benzyloxy-4-(methoxycarbonylmethylamino)-phenoxy]-acetic acid 2-trimethylsilanylethyl ester (5.35 g, 12 mmol) and triethylamine (2.07 g, 20.4 mmol) in methylene chloride (15 mL) and the mixture is stirred at RT for 2 h. The mixture is washed with water and the organic phase is dried over NaSO4. The solvent is removed under reduced pressure and the residue is purified by column chromatography to using EtOAc/hexane (3:7) as eluent to give the title compound.

後処理

  1. customis allowed to wart to RT
  2. stirringthe mixture is stirred at RT for 2 h
  3. washThe mixture is washed with water
  4. dry with materialthe organic phase is dried over NaSO4
  5. customThe solvent is removed under reduced pressure
  6. customthe residue is purified by column chromatography

出典と根拠

ORDレコード
ord-776ac560788640c5850223160dedd333
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08084448B2

反応ノート

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