Diethoxymethane → 4-(Ethoxymethoxy)-1,1,2,3,3-pentamethyloctahydro-1H-indene

HRID 348507

반응식

HRID 348507 반응식
[CH3:1][C:2]1([CH3:15])[CH:10]2[CH:5]([CH:6]([OH:11])[CH2:7][CH2:8][CH2:9]2)[C:4]([CH3:13])([CH3:12])[CH:3]1[CH3:14].[CH2:16]([O:18][CH2:19]OCC)[CH3:17]>C1(C)C=CC=CC=1>[CH3:1][C:2]1([CH3:15])[CH:10]2[CH:5]([CH:6]([O:11][CH2:19][O:18][CH2:16][CH3:17])[CH2:7][CH2:8][CH2:9]2)[C:4]([CH3:13])([CH3:12])[CH:3]1[CH3:14]

참가 물질

4

반응물 2

HCID 10024DiethoxymethaneHCID 210875771,1,2,3,3-Pentamethyl-hexahydro-4-indanol

생성물 1

HCID 210875784-(Ethoxymethoxy)-1,1,2,3,3-pentamethyloctahydro-1H-indene수율 68.1%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
100 °C

실험 절차

A reaction flask was charged with 300 g (1.4 mole) 1,1,2,3,3-pentamethyl-hexahydro-4-indanol, 258 g (2.5 mole) diethoxymethane, 0.25 liter toluene, and 5 g boron trifluoride etherate complex. The reaction mass was heated to 100° C. and methanol and lite organics were collected in a Dean Stark trap (190 g recovered). After aging the reaction for 2 hrs the reaction was cooled to 25° C. and acid catalyst was quenched with 100 g of 10% aqueous sodium carbonate. The mass was transferred to a separatory funnel and water washed. The organic layer was separated and purified by fractional distillation. The procedure afforded a 68% yield (256 g) of 1,1,2,3,3-pentamethyl-octahydro-4-(ethoxymethoxy)-1H-indene.

후처리

  1. custommethanol and lite organics were collected in a Dean Stark trap (190 g recovered)
  2. customthe reaction for 2 hrs the reaction
  3. temperaturewas cooled to 25° C.
  4. customacid catalyst was quenched with 100 g of 10% aqueous sodium carbonate
  5. customThe mass was transferred to a separatory funnel
  6. washwater washed
  7. customThe organic layer was separated
  8. distillationpurified by fractional distillation

출처 및 근거

ORD 기록
ord-5c1f3ef50c8146ed8cad4d29d17191f0
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07176324B1

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