Water → HCID 21397385, 화합물

HRID 1439485노트

반응식

HRID 1439485 반응식
[H-].[Na+].[C:3]1([CH:9]([CH2:13][CH2:14][CH2:15][CH:16]([O:22][CH2:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])[C:10](=[O:12])[CH3:11])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.Br[CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][C:37]([O:39][CH2:40][CH3:41])=[O:38].O>C1C=CC=CC=1.CN(C)C=O.CCOCC>[C:10]([C:9]([C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1)([CH2:13][CH2:14][CH2:15][CH:16]([O:22][CH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)[CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])[CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][C:37]([O:39][CH2:40][CH3:41])=[O:38])(=[O:12])[CH3:11]

참가 물질

8

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 122490Ethyl 7-bromoheptanoateHCID 213973967-(Benzyloxy)-3-phenyldodecan-2-one

생성물 1

HCID 21397385HCID 21397385, 화합물

시약·촉매·용매 3

HCID 241Benzene용매HCID 3283Diethyl Ether용매HCID 6228Dimethylformamide용매

실험 절차

Sodium hydride (0.8 g., 0.033 mole) is suspended in a mixture of benzene (50 ml.) and dimethylformamide (50 ml.) and 3-phenyl-7-benzyloxy-2-dodecanone (12.1 g., 0.033 mole) is added dropwise. The resulting mixture is heated on the steam bath for one hour and then cooled to room temperature. Ethyl 7-bromoheptanoate (8.8 g., 0.037 mole) is added dropwise and the mixture is heated on the steam bath for 24 hours. The reaction mixture is cooled, poured into water (200 ml.) and the oily product taken up into ether and dried over sodium sulfate. The solvent is distilled in vacuo to leave 14 g. of ethyl 8-acetyl-8-phenyl-12-benzyloxyheptadecanoate as a yellow oil which is used in Step G without further purification.

후처리

  1. additionis added dropwise
  2. temperatureThe resulting mixture is heated on the steam bath for one hour
  3. temperaturethe mixture is heated on the steam bath for 24 hours
  4. temperatureThe reaction mixture is cooled
  5. dry with materialdried over sodium sulfate
  6. distillationThe solvent is distilled in vacuo
  7. customto leave 14 g
  8. customof ethyl 8-acetyl-8-phenyl-12-benzyloxyheptadecanoate as a yellow oil which is used in Step G without further purification

출처 및 근거

ORD 기록
ord-d7c6813ddfbd4da783827837d3c4ec7f
출처 데이터셋
uspto-grants-1977_11
특허 번호
US04059602

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