Iodine → 1-Benzyloxy-3-iodopropane

HRID 1758167ノート

反応式

HRID 1758167 の反応式
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

参加物

7

反応物 4

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

生成物 1

HCID 104686631-Benzyloxy-3-iodopropane収率 53%

試薬・触媒・溶媒 2

HCID 241Benzene溶媒2 回HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-00ae948dc5c7426fadb8151c24bc7583
出典データセット
uspto-grants-1983_02
特許番号
US04371720

反応ノート

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