1,2-Benzenedimethanol → N,N-Diisopropyl-1,5-dihydrobenzo[e][1,3,2]dioxaphosphepin-3-amine

HRID 258157

反応式

HRID 258157 の反応式
[OH:1][CH2:2][C:3]1[C:4](=[CH:7][CH:8]=[CH:9][CH:10]=1)[CH2:5][OH:6].[CH:11]([N:14]([P:18](N(C(C)C)C(C)C)Cl)[CH:15]([CH3:17])[CH3:16])([CH3:13])[CH3:12]>C1COCC1>[CH:11]([N:14]([CH:15]([CH3:17])[CH3:16])[P:18]1[O:6][CH2:5][C:4]2[CH:7]=[CH:8][CH:9]=[CH:10][C:3]=2[CH2:2][O:1]1)([CH3:13])[CH3:12]

参加物

4

反応物 2

HCID 691531,2-Benzenedimethanol2 回HCID 2733425Bis(diisopropylamino)chlorophosphine

生成物 1

HCID 19782585N,N-Diisopropyl-1,5-dihydrobenzo[e][1,3,2]dioxaphosphepin-3-amine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Phthalyl alcohol (1.15 g, 8.31 mmol) was dissolved in 5 ml of THF, and bisdiisopropylaminochlorophosphine (2.21 g, 8.31 mmol) which was dissolved in 5 ml of THF was added dropwise to the solution at -15° C. under a nitrogen atmosphere. Afterward, the temperature of the solution was adjusted to room temperature, and after the disappearance of phthalyl alcohol had been confirmed, hydrochloride of diisopropylamine was washed with ether. The wash liquor was concentrated and then distilled in order to obtain the desired product having a melting point of from 150° to 155° C. (0.7 mmHg).

後処理

  1. additionwas added dropwise to the solution at -15° C. under a nitrogen atmosphere
  2. customwas adjusted to room temperature
  3. washhydrochloride of diisopropylamine was washed with ether
  4. concentrationThe wash liquor was concentrated
  5. distillationdistilled in order

出典と根拠

ORDレコード
ord-9d568a1daaed4c6d917cab90fc95f644
出典データセット
uspto-grants-1993_11
特許番号
US05264605

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