Iodine → GDMA 3-methyl-3-butene-1-ol

HRID 382656

반응식

HRID 382656 반응식
[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]

참가 물질

4

반응물 3

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

생성물 1

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

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2523c360ebf24338896ceda6eb074615
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06310161B1

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