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

HRID 258157

반응식

HRID 258157 반응식
[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]

참가 물질

4

반응물 2

HCID 691531,2-Benzenedimethanol2회HCID 2733425Bis(diisopropylamino)chlorophosphine

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-9d568a1daaed4c6d917cab90fc95f644
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05264605

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