Ethylenediamine → alpha-Thujene

HRID 1758592

반응식

HRID 1758592 반응식
[Li].C(N)CN.[CH3:6][CH:7]([C:9]12[CH2:15][CH:14]1[C:12](=[CH2:13])[CH2:11][CH2:10]2)[CH3:8].CC([C@@]12C[C@@H]1C(=C)CC2)C>>[CH3:13][C:12]1[CH:14]2[CH2:15][C:9]2([CH:7]([CH3:8])[CH3:6])[CH2:10][CH:11]=1

참가 물질

5

반응물 4

HCID 3301EthylenediamineHCID 18818SabineneHCID 3028194LithiumHCID 10887971(+)-Sabinene

생성물 1

HCID 17868alpha-Thujene수율 69.3%

실험 절차

0.48 g (69 millimoles) of lithium and 9 g (150 millimoles) of ethylenediamine were reacted in the atmosphere of air at a temperature of 128°-133° C. for 4 hours, and then mixed with 82 g of the above-prepared sabinene oil containing 35.7 g (262 millimoles) of (+)-sabinene. The mixture was allowed to react for 6 hours at 130° C. The reaction mixture was treated as described in Example 1 and thereafter, subjected to distillation at 60°-75° C. and 30 mmHg, affording 56.8 g of α-thujene oil containing 47.8% of (-)-α-thujene. The yield of (-)-α-thujene was 76.0%.

후처리

  1. customto react for 6 hours at 130° C
  2. additionThe reaction mixture was treated
  3. distillationsubjected to distillation at 60°-75° C.

출처 및 근거

ORD 기록
ord-e7073b02230649dd8732239c2c2cacba
출처 데이터셋
uspto-grants-1983_02
특허 번호
US04374292

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