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Triethylamine → HCID 22228407, 화합물

HRID 1795164
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HRID 1795164 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[C:6]([O:10][C:11]([N:13]1[CH2:18][CH2:17][C:16]([CH:21]2[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]2)([CH2:19][OH:20])[CH2:15][CH2:14]1)=[O:12])([CH3:9])([CH3:8])[CH3:7].C(N(CC)CC)C>ClCCl>[C:6]([O:10][C:11]([N:13]1[CH2:14][CH2:15][C:16]([CH:21]2[CH2:22][CH2:23][CH2:24][CH2:25][CH2:26]2)([CH2:19][O:20][S:2]([CH3:1])(=[O:4])=[O:3])[CH2:17][CH2:18]1)=[O:12])([CH3:9])([CH3:7])[CH3:8]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 11000987HCID 11000987, 화합물

생성물 1

HCID 22228407HCID 22228407, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Methane sulfonyl chloride (1.8 mL, 23.0 mmol) is added to a stirred solution of 4-cyclohexyl-4-hydroxymethylpiperidine-1-carboxylic acid tert-butyl ester, 3, (3.42 g, 11.48 mmol) and triethylamine (4.8 mL, 2.8 mmol) in dichloromethane (30 mL) at 0° C. The reaction mixture is then allowed to warm to room temperature and stir for 1 hour. The reaction is quenched with a saturated solution of NaHCO3 and the resulting mixture is extracted twice with dichloromethane (50 mL). The organic layers are combined, dried, filtered and concentrated in vacuo to yield the desired product in quantitative yield. The material is used for the next step without need for purification.

후처리

  1. customThe reaction is quenched with a saturated solution of NaHCO3
  2. extractionthe resulting mixture is extracted twice with dichloromethane (50 mL)
  3. customdried
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-c44161145743428585398332d8ac9353
출처 데이터셋
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07026335B2

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