Triethylamine → HCID 66765157、化合物

HRID 577268ノート

反応式

HRID 577268 の反応式
[CH3:1][C:2]1[C:7]([N:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:14]O.C(N(CC)CC)C.S([Cl:27])(C)(=O)=O>C(Cl)Cl>[Cl:27][CH2:14][C:3]1[C:2]([CH3:1])=[C:7]([N:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)[CH:6]=[CH:5][CH:4]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 67112254HCID 67112254、化合物

生成物 1

HCID 66765157HCID 66765157、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

(2-methyl-3-morpholinophenyl)methanol (0.468 g, 2.26 mmol) was dissolved in dry DCM (14 mL) with triethylamine (0.669 mL, 4.82 mmol) and this stirred solution was cooled at 0° C. in an ice bath. Mesyl chloride (0.415 g, 3.62 mmol) was added dropwise and the reaction was allowed to reach rt overnight. The mixture was diluted in DCM (25 mL), washed with water (20 mL) and the water re-extracted with DCM (20 mL). The combined organics were dried over Na2SO4, filtered and the solvent removed under vacuum to afford 4-(3-(chloromethyl)-2-methylphenyl)morpholine as a crude oil (0.5 g, 98% yield).

後処理

  1. washwashed with water (20 mL)
  2. extractionthe water re-extracted with DCM (20 mL)
  3. dry with materialThe combined organics were dried over Na2SO4
  4. filtrationfiltered
  5. customthe solvent removed under vacuum

出典と根拠

ORDレコード
ord-b03127007bbb4e789dffdf0cf30c772b
出典データセット
uspto-grants-2015_05
特許番号
US09040545B2

反応ノート

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