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Methyl Bromide → Tris(4-hydroxyphenyl)phosphine oxide

HRID 967681
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HRID 967681 반응식
C[O:2][C:3]1[CH:8]=[CH:7][C:6]([P:9](=[O:26])([C:18]2[CH:23]=[CH:22][C:21]([O:24]C)=[CH:20][CH:19]=2)[C:10]2[CH:15]=[CH:14][C:13]([O:16]C)=[CH:12][CH:11]=2)=[CH:5][CH:4]=1.[K+].[Br-].S([O-])([O-])=O.[Na+].[Na+].CBr>Br>[OH:2][C:3]1[CH:4]=[CH:5][C:6]([P:9](=[O:26])([C:10]2[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][CH:11]=2)[C:18]2[CH:19]=[CH:20][C:21]([OH:24])=[CH:22][CH:23]=2)=[CH:7][CH:8]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6323Methyl BromideHCID 24437Sodium SulfiteHCID 253877Potassium BromideHCID 3057506Tris(4-methoxyphenyl)phosphine oxide

생성물 1

HCID 4183961Tris(4-hydroxyphenyl)phosphine oxide수율 64.8%

시약·촉매·용매 1

HCID 260Hydrogen Bromide
용매

반응 조건

온도
114 °C

실험 절차

A reaction flask containing tris(4-methoxyphenyl)phosphine oxide (973.2 g) was charged with 48% aq HBr (2250 mL) and KBr (126.1 g). The flask was fitted with a sodium sulfite scrubber for containment of methyl bromide. The reaction mixture was heated to reflux (114° C.) and maintained at reflux until complete based on HPLC analysis. The product was worked up to give 558.5 g of tris(4-hydroxyphenyl)phosphine oxide (31P NMR (d6-DMSO): δ 27.6 (s); 1H NMR (d6-DMSO): δ 10.9 (s, 3H), 7.38 (m, 6H), 6.84 (m, 6H)).

후처리

  1. temperatureThe reaction mixture was heated
  2. temperaturemaintained
  3. temperatureat reflux

출처 및 근거

ORD 기록
ord-c70a4220ad104c6e99a5829a82b32426
출처 데이터셋
uspto-grants-2005_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06955851B2

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