Lauryldimethylamine → HCID 22111399、化合物

HRID 565586

反応式

HRID 565586 の反応式
[CH3:1][N:2]([CH3:15])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].[Cl:16][CH2:17][S:18][C:19]#[N:20]>O1CCCC1>[Cl-:16].[CH3:1][N+:2]([CH3:15])([CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14])[CH2:17][S:18][C:19]#[N:20]

参加物

4

反応物 2

HCID 8168LauryldimethylamineHCID 76755Thiocyanic acid, chloromethyl ester

生成物 1

HCID 22111399HCID 22111399、化合物収率 79.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A 2 liter flask was charged with 1 liter of tetrahydrofuran, 277 g of dimethyldodecylamine and then 153.7 g of chloromethylthiocyanate. The reaction mixture was stirred at ambient temperature for 17 hours. A considerable amount of solids was formed. The reaction was then stirred for 7 more hours at 35° C. The solid was filtered off with suction and the solid washed with diethyl ether. The filtrate now formed more solid which was filtered off, washed with ether and then combined with the other solid. The combined solids were now allowed to air dry to constant weight, 331.0 g, for a 79.4% yield. Analysis (nmr) showed a purity of better than 98%.

後処理

  1. customA considerable amount of solids was formed
  2. stirringThe reaction was then stirred for 7 more hours at 35° C
  3. filtrationThe solid was filtered off with suction
  4. washthe solid washed with diethyl ether
  5. customThe filtrate now formed more solid which
  6. filtrationwas filtered off
  7. washwashed with ether
  8. customto air dry to constant weight, 331.0 g, for a 79.4% yield

出典と根拠

ORDレコード
ord-eb7a11205d7645a18d93c723d47218df
出典データセット
uspto-grants-2001_01
特許番号
US06172117B2

関連ノート

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