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Triethylamine → HCID 22557737, 화합물

HRID 984063
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HRID 984063 반응식
[C:1]([OH:4])(=[O:3])[CH3:2].[NH2:5][C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][C:11]=1[O:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.C(N(CC)CC)C.[CH2:27]([S:31](Cl)(=[O:33])=[O:32])[CH2:28][CH2:29][CH3:30]>C(Cl)Cl>[C:1]([OH:4])(=[O:3])[CH3:2].[CH2:13]([O:12][C:11]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[NH:5][S:31]([CH2:27][CH2:28][CH2:29][CH3:30])(=[O:33])=[O:32])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 754301-Butanesulfonyl chlorideHCID 69680486HCID 69680486, 화합물

생성물 1

HCID 22557737HCID 22557737, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
30 °C

실험 절차

5.0 g (0.00194 mol) of 3-amino-4-benzyloxybenzene acetate are mixed under a nitrogen atmosphere in 15 ml of methylene chloride, and 3.3 ml of triethylamine (0.0236 mol) and 3.3 ml (0.0245 mol) of 1-butansulfonyl chloride are added thereto. The mixture is stirred at ambient temperature overnight and afterwards at 30° C. for 4 hours. Washing with water is carried out, the two phases are separated, the organic phase is dried over sodium sulfate and filtered, and the solvent is evaporated under reduced pressure. Purification is carried out by chromatography on a column of silica gel, elution being carried out with a cyclohexane/ethyl acetate=9:1 mixture. The title compound is obtained.

후처리

  1. washWashing with water
  2. customthe two phases are separated
  3. dry with materialthe organic phase is dried over sodium sulfate
  4. filtrationfiltered
  5. customthe solvent is evaporated under reduced pressure
  6. customPurification
  7. washis carried out by chromatography on a column of silica gel, elution

출처 및 근거

ORD 기록
ord-a577057633374760970b46baa227988a
출처 데이터셋
uspto-grants-2005_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06867220B2

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