Iodine → 1-Benzyloxy-3-iodopropane

HRID 1650062노트

반응식

HRID 1650062 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[I:20]I.N1C=CC=CC=1.[CH2:28]([O:35][CH2:36][CH2:37][CH2:38]O)[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1>CO.C1C=CC=CC=1>[CH2:28]([O:35][CH2:36][CH2:37][CH2:38][I:20])[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1

참가 물질

7

반응물 4

HCID 807IodineHCID 1049PyridineHCID 11776TriphenylphosphineHCID 3479713-Benzyloxy-1-propanol

생성물 1

HCID 104686631-Benzyloxy-3-iodopropane수율 53%

시약·촉매·용매 2

HCID 241Benzene용매2회HCID 887Methanol용매

실험 절차

To a solution of 83.3 g. (0.318 mole) triphenylphosphine in 200 ml. benzene was added, in four portions, 80 g. (0.318 mole) of iodine. The resultant mixture was stirred 3 hours and then 50 ml. (0.618 mole) of pyridine was added followed by the slow addition of 32 g. (0.192 mole) of 3-benzyloxypropanol in 250 ml. of benzene. The reaction was stirred 15 hours longer and then diluted with 40 ml. of methanol. The mixture was filtered through diatomaceous earth and the filtrate evaporated to an oil. Distillation of the crude oil yielded 28 g. (53%) of the title compound as an oil.

후처리

  1. additionfollowed by the slow addition of 32 g
  2. additiondiluted with 40 ml
  3. filtrationThe mixture was filtered through diatomaceous earth
  4. customthe filtrate evaporated to an oil
  5. distillationDistillation of the crude oil
  6. customyielded 28 g

출처 및 근거

ORD 기록
ord-323b0e99c2cf4678ab21ca70e07ba691
출처 데이터셋
uspto-grants-1990_05
특허 번호
US04921994

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