2,2,6,6-Tetramethylpiperidine → HCID 12951849, 화합물

HRID 2058661노트

반응식

HRID 2058661 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([F:10])=[C:6]([CH:9]=1)[CH2:7]Br.[CH3:11][NH:12][CH2:13][CH2:14][CH:15]([OH:22])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.CC1(C)CCCC(C)(C)N1>C(#N)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([F:10])=[C:6]([CH2:7][N:12]([CH2:13][CH2:14][CH:15]([OH:22])[C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH3:11])[CH:9]=1

참가 물질

5

반응물 3

HCID 130352,2,6,6-TetramethylpiperidineHCID 27339893-Methylamino-1-phenylpropanolHCID 27736262-(Bromomethyl)-4-chloro-1-fluorobenzene

생성물 1

HCID 12951849HCID 12951849, 화합물수율 73.2%

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

A solution of 5-chloro-2-fluorobenzyl bromide (10.5 g) in acetonitrile (100 ml) was added dropwise to a mixture of N-methyl-3-hydroxy-3-phenylpropylamine (7.7 g), 2,2,6,6-tetramethylpiperidine (8 ml) and acetonitrile (100 ml). After 12h the mixture was filtered, and filtrate evaporated and the residue chromatographed on silica (Woelm Grade 1) using ether as eluant to give the title compound as an oil (10.5 g), b.p. 160°/0.5 mm. (Found: C, 66.1; H, 6.2; N, 4.1%; C17H19ClFNO requires: C, 66.3; H, 6.2; N, 4.55%).

후처리

  1. filtrationAfter 12h the mixture was filtered
  2. customfiltrate evaporated
  3. customthe residue chromatographed on silica (Woelm Grade 1)

출처 및 근거

ORD 기록
ord-588a8b1336a541ee860dcc8dddfc9a32
출처 데이터셋
uspto-grants-1982_03
특허 번호
US04318909

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