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tert-Butanol → HCID 68997226, 화합물

HRID 660763
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HRID 660763 반응식
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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

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6

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HCID 6386tert-ButanolHCID 8471TriethylamineHCID 70918Chlorosulfonyl isocyanateHCID 68838279HCID 68838279, 화합물

생성물 1

HCID 68997226HCID 68997226, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-776ac560788640c5850223160dedd333
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08084448B2

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