2,2,6,6-Tetramethylpiperidine → HCID 12951849、化合物

HRID 2058661ノート

反応式

HRID 2058661 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 12951849HCID 12951849、化合物収率 73.2%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-588a8b1336a541ee860dcc8dddfc9a32
出典データセット
uspto-grants-1982_03
特許番号
US04318909

反応ノート

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