Triethylamine → HCID 67683117, 화합물

HRID 260337노트

반응식

HRID 260337 반응식
Cl.[CH2:2]1[C:6]2([CH2:11][CH2:10][NH:9][CH2:8][CH2:7]2)[CH2:5][CH2:4][CH2:3]1.C(N(CC)CC)C.[O:19]([C:26]1[CH:31]=[CH:30][C:29]([O:32][C:33]([NH:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][O:42][C:43]([N:45]2[CH2:50][CH2:49][CH:48]([O:51][C:52](OC3C=CC([N+]([O-])=O)=CC=3)=[O:53])[CH2:47][CH2:46]2)=[O:44])=[O:34])=[CH:28][CH:27]=1)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>CN(C)C=O.C(OCC)(=O)C>[O:19]([C:26]1[CH:31]=[CH:30][C:29]([O:32][C:33]([NH:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][O:42][C:43]([N:45]2[CH2:50][CH2:49][CH:48]([O:51][C:52]([N:9]3[CH2:10][CH2:11][C:6]4([CH2:5][CH2:4][CH2:3][CH2:2]4)[CH2:7][CH2:8]3)=[O:53])[CH2:47][CH2:46]2)=[O:44])=[O:34])=[CH:28][CH:27]=1)[C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 152933074-(4-Nitro-phenoxycarbonyloxy)-piperidine-1-carboxylic acid 6-[(4-phenoxy-phenyl)-oxycarbonylamino]-hexyl esterHCID 224012298-Azaspiro(4.5)decane hydrochloride

생성물 1

HCID 67683117HCID 67683117, 화합물수율 82.4%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매2회HCID 8857Ethyl Acetate용매

실험 절차

A solution of 8-aza-spiro[4.5]decane hydrochloride (791 mg, 4.50 mmol) and triethylamine (2.24 mL, 16.1 mmol) in 20 mL of anhydrous dimethylformamide was added under nitrogen dropwise to a solution of the carbonate prepared in Example 5 (2.00 g, 3.22 mmol) in 25 mL of anhydrous dimethylformamide. After the addition the reaction was stirred at room temperature overnight. The reaction was diluted with ethyl acetate, extracted one time with 1N HCl, multiple times with saturated Na2CO3 and then water, dried (MgSO4) and the solvent removed under reduced pressure to give 1.65 g of an oil. Purification of the oil on silica gel (230-400 mesh) using 20% ethyl acetate-methylene chloride as the eluent gave 1.01 g (52%) of the title compound as a light yellow oil, MS [M+H]+ 622.

후처리

  1. additionAfter the addition the reaction
  2. extractionextracted one time with 1N HCl, multiple times with saturated Na2CO3
  3. dry with materialwater, dried (MgSO4)
  4. customthe solvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-81abfca44c954bb2a48ed2365b50d137
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05527804

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