Triethylamine → (3-(Tert-butoxycarbonylamino)cyclohexyl)methyl methanesulfonate

HRID 530868노트

반응식

HRID 530868 반응식
[OH:1][CH2:2][CH:3]1[CH2:8][CH2:7][CH2:6][CH:5]([NH:9][C:10](=[O:16])[O:11][C:12]([CH3:15])([CH3:14])[CH3:13])[CH2:4]1.[CH3:17][S:18](Cl)(=[O:20])=[O:19].C(N(CC)CC)C>C(Cl)Cl>[CH3:17][S:18]([O:1][CH2:2][CH:3]1[CH2:8][CH2:7][CH2:6][CH:5]([NH:9][C:10]([O:11][C:12]([CH3:13])([CH3:15])[CH3:14])=[O:16])[CH2:4]1)(=[O:20])=[O:19]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 22106830tert-butyl N-[3-(hydroxymethyl)cyclohexyl]carbamate

생성물 1

HCID 86698246(3-(Tert-butoxycarbonylamino)cyclohexyl)methyl methanesulfonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of tert-butyl 3-(hydroxymethyl)cyclohexylcarbamate (7.9 mmol), methanesulfonyl chloride (23.7 mmol) and triethylamine (119 mmol) in DCM (100 ml) was stirred at rt overnight. The reaction was quenched with water (50 mL) and extracted with ethyl acetate (3×100 mL). The extracts were combined, dried using anhydrous sodium sulfate, filtered, and concentrated in vacuo. The crude product was progressed to the next step without purification.

후처리

  1. customThe reaction was quenched with water (50 mL)
  2. extractionextracted with ethyl acetate (3×100 mL)
  3. customdried
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe crude product was progressed to the next step without purification

출처 및 근거

ORD 기록
ord-ddf801520ebc4283a3e6da4f3cd0ae16
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09351965B2

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