Triethylamine → HCID 20031878, 화합물

HRID 2291293노트

반응식

HRID 2291293 반응식
[C:1]([Cl:4])(Cl)=[S:2].[OH:5][C:6]1[CH:7]=[C:8]([CH:29]=[CH:30][CH:31]=1)[C:9]([O:11][Si:12]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[C:13]([CH3:16])([CH3:15])[CH3:14])=[O:10].C(N(CC)CC)C>C(OCC)C>[Cl:4][C:1]([O:5][C:6]1[CH:7]=[C:8]([CH:29]=[CH:30][CH:31]=1)[C:9]([O:11][Si:12]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[C:13]([CH3:16])([CH3:14])[CH3:15])=[O:10])=[S:2]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 10040ThiophosgeneHCID 54284754HCID 54284754, 화합물

생성물 1

HCID 20031878HCID 20031878, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

반응 조건

온도
-78 °C

실험 절차

To a stirred solution of 130 ml of thiophosgene in 250 ml of dry diethyl ether at -78° C. was added dropwise a mixture of 72 g of diphenyl- (2-methylprop-2-yl)silyl 3-hydroxybenzoate and 29 ml of triethylamine in 200 ml of dry diethyl ether. The mixture was stirred at -78° C. for 30 minutes, at room temperature for 120 minutes, and then partitioned between diethyl ether and water. The organic layer was washed with cold water and with brine, and was dried over anhydrous calcium chloride. Evaporation in vacuo, and repeated addition of dry diethyl ether and re-evaporation in vacuo afforded 86.5 g of the title compound as a viscous orange oil.

후처리

  1. custompartitioned between diethyl ether and water
  2. washThe organic layer was washed with cold water and with brine
  3. dry with materialwas dried over anhydrous calcium chloride
  4. customEvaporation in vacuo
  5. additionaddition of dry diethyl ether and re-evaporation in vacuo

출처 및 근거

ORD 기록
ord-89028ea92ee2488eb6c9d0a867eb72f1
출처 데이터셋
uspto-grants-1989_01
특허 번호
US04795748

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