Iodine → GDMA 3-methyl-3-butene-1-ol

HRID 382656

反応式

HRID 382656 の反応式
[CH2:1]([O:8][C:9]([CH2:11][SH:12])=[O:10])[CH2:2][O:3][C:4]([CH2:6][SH:7])=[O:5].[CH3:13][C:14](=[CH2:18])[CH2:15][CH2:16][OH:17].II>>[CH2:2]([O:3][C:4]([CH2:6][SH:7])=[O:5])[CH2:1][O:8][C:9]([CH2:11][SH:12])=[O:10].[CH3:18][C:14](=[CH2:13])[CH2:15][CH2:16][OH:17]

参加物

4

反応物 3

HCID 807IodineHCID 129883-Methyl-3-buten-1-olHCID 61059Ethylene di(S-thioacetate)

生成物 1

HCID 131722937GDMA 3-methyl-3-butene-1-ol

反応条件

温度
60 °C

実験手順

The flask was set up for reaction and agitation as described in Example 6. No heat was initially added to the flask containing the GDMA. The addition funnel containing the 3-methyl-3-butene-1-ol was placed on the second neck of the flask and a slow drip was started. The reaction exotherm was mild and the addition was completed in 40 minutes. The flask was then heated to 60° C. and held for one hour. Iodine titration indicated a significant amount of free thiol remaining (3.72 meq/g). Lupersol 575 (2.5 g) was added slowly. A significant exotherm occurred, after which the free thiol was measured to be 0.047 meq/gram. The material was then stored in dark high density polyethylene bottles.

後処理

  1. customThe flask was set up for reaction and agitation
  2. additionNo heat was initially added to the flask
  3. additionthe addition
  4. waitheld for one hour

出典と根拠

ORDレコード
ord-2523c360ebf24338896ceda6eb074615
出典データセット
uspto-grants-2001_10
特許番号
US06310161B1

関連ノート

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